CN115636677B - Tin bath top cover brick for float glass production and preparation method thereof - Google Patents
Tin bath top cover brick for float glass production and preparation method thereof Download PDFInfo
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- CN115636677B CN115636677B CN202211320229.4A CN202211320229A CN115636677B CN 115636677 B CN115636677 B CN 115636677B CN 202211320229 A CN202211320229 A CN 202211320229A CN 115636677 B CN115636677 B CN 115636677B
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- 239000011449 brick Substances 0.000 title claims abstract description 68
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000005329 float glass Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052849 andalusite Inorganic materials 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004568 cement Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- 239000011707 mineral Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052656 albite Inorganic materials 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910052642 spodumene Inorganic materials 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 15
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 8
- 235000010755 mineral Nutrition 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011819 refractory material Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 235000012255 calcium oxide Nutrition 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000006124 Pilkington process Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011221 initial treatment Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052851 sillimanite Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Abstract
The application provides a tin bath top cover brick for float glass production and a preparation method thereof, wherein the tin bath top cover brick comprises the following raw material components in percentage by mass: 60-74% of andalusite aggregate, 10-15% of andalusite fine powder, 4-9% of pure calcium aluminate cement, 3-9% of alumina micropowder, 3-8% of sol, 0.1-5% of silica micropowder, 0.1-3% of glass phase forming agent and 0.1-0.5% of water reducer. The preparation method comprises the steps of preparing prefabricated materials, preparing mixed powder, preparing the mixed materials, casting, demoulding, curing and calcining at high temperature to obtain the tin bath top cover brick. The application can improve the thermal stability, corrosion resistance and thermal shock resistance of the prepared tin bath top cover brick, and simultaneously reduce the thermal conductivity of the tin bath top cover brick.
Description
Technical Field
The application relates to the technical field of refractory materials, in particular to a tin bath top cover brick for float glass production and a preparation method thereof.
Background
Glass is one of important materials for supporting national economic development, and is widely applied to the fields of construction, transportation, furniture home appliances, instruments, aerospace, nuclear engineering and the like. Currently, the main process for producing glass is the float glass process. Tin baths are key devices for glass production in the float glass process, which play a critical role in glass quality control.
The tin bath is mainly composed of a bath bottom and a top cover (the top cover is formed by piling bricks on the top cover), and when the molten glass at 1100-1200 ℃ flows into the surface of the tin bath bottom from the kiln, na is contained 2 O、H 2 The S and other aggressive gases are also carried into the tin bath, so that refractory materials in the tin bath top cover bricks can be seriously eroded and dripping matters are generated, and the yield and quality of glass are greatly influenced; and after the top cover is corroded, the top cover is locally thinned, so that heat dissipation is uneven, heat preservation performance and heat efficiency are reduced, the cooling temperature of glass liquid is difficult to control, poor thickness adjustment of glass finished products is affected, glass output quality is reduced, and energy consumption of a glass melting furnace is improved.
In addition, the thermal shock resistance of the top cover of most of the current tin baths is poor, cracks are very easy to generate, the area and depth of gas erosion are increased, the service life of the top cover is shortened, and the economical efficiency is lower. Therefore, the choice of the tin bath roof structure and refractory material is very important, which directly relates to the quality of the glass and the service life of the tin bath.
In view of the above problems, countermeasures currently taken are broadly classified into the following two categories:
one type is to change the structure of the tin bath roof. For example, patent CN 202246389a proposes a combined roof tile structure with arch shape, which makes the vertical distance between the bottom of the tin bath and the roof tile gradually decrease from the edge to the middle, solves the problem of uneven heat dissipation at the edge of the tin bath, reduces the energy consumption of the tin bath, but still can be eroded by part of gas in the use process. The tin bath top cover is formed by laminating refractory bricks and insulating bricks in the patent CN210764973U and the patent CN 213388337U, so that the corrosion resistance of the top cover is enhanced, but the superposition of the multi-layer bricks can increase the weight of the top cover, and the construction is difficult and the safety is lower.
The other is to develop erosion resistant refractory materials as the raw material for the tin bath roof bricks. For example, mullite capping bricks disclosed in patent CN 104326755A, calcia capping bricks disclosed in patent CN 112194345A, and sillimanite thermal bricks disclosed in patent CN112159080a and the like special for tin bath capping bricks, such refractory capping bricks have poor erosion resistance at high temperature and poor thermal shock resistance, are extremely easy to generate cracks when temperature changes are large, aggressive gas enters the cracks to increase erosion contact surfaces, cause larger-area cracking, and even generate partial glass phase and slag drop on a tin bath, so that the quality of glass is seriously affected.
In summary, the main problems of the existing tin bath top cover bricks are poor thermal stability and weak corrosion resistance, and cracking and glass phase and slag dripping are easy to occur.
Disclosure of Invention
The application aims to provide a tin bath top cover brick for float glass production and a preparation method thereof, and the refractory raw materials are combined in raw material components, so that the heat stability, corrosion resistance and thermal shock resistance of the tin bath top cover brick are improved, and the heat conductivity of the tin bath top cover brick is reduced. The specific technical scheme is as follows:
in a first aspect, the application provides a tin bath roof brick for float glass production, which comprises the following raw material components in percentage by mass: 60-74% of andalusite aggregate, 10-15% of andalusite fine powder, 4-9% of pure calcium aluminate cement, 3-9% of alumina micropowder, 3-8% of sol, 0.1-5% of silica micropowder, 0.1-3% of glass phase forming agent and 0.1-0.5% of water reducer.
Further, the andalusite aggregate and the andalusite fine powder comprise the following components in percentage by mass: al (Al) 2 O 3 The mass percentage of (2) is more than or equal to 58 percent, fe 2 O 3 Is less than or equal to 0.5 percent of Na by mass 2 O, mgO and K 2 The sum of the mass percentages of O is less than or equal to 0.5 percent.
Further, the sol is at least one of silica sol, aluminum sol and silicon aluminum sol.
Further, the glass phase forming agent comprises at least one of spodumene, albite and a mixture of potassium-sodium containing minerals (including a mixture of minerals such as sodium carbonate and potassium carbonate).
Further, the pure calcium aluminate cement comprises the following components in percentage by mass: al (Al) 2 O 3 70-80% by mass and 20-30% by mass of CaO;
the alumina micropowder is alpha-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein, the mass percent is alpha-Al 2 O 3 The purity of (2) is greater than 99%;
in the silicon micropowder, siO 2 The mass percentage content of (2) is more than or equal to 95 percent;
the water reducer comprises at least one of sodium tripolyphosphate, sodium polyacrylate and sodium hexametaphosphate.
Further, the particle size of the andalusite aggregate is less than or equal to 5mm; the grain size of the andalusite fine powder is 200-325 meshes; the granularity of the pure calcium aluminate cement is not more than 300 meshes; the grain diameter of the alumina micropowder is 2-5 mu m; the particle size of the silicon micropowder is 0.3-2 μm.
In a second aspect, the application provides a method for preparing the tin bath roof brick for float glass production, which comprises the following steps:
step S1, preparing a prefabricated material
Weighing andalusite fine powder and sol with required mass percentages, stirring and uniformly mixing, heating to about 1200-1600 ℃, preserving heat for 1-4 hours, stopping heating, cooling to room temperature, taking out, and placing in a ball mill for grinding until the particle size is 5-25 microns, thereby preparing a prefabricated material;
s2, preparing mixed powder
Weighing the pure calcium aluminate cement, the alumina micropowder, the silica micropowder, the water reducer and the glass phase forming agent which are in the required mass percentage, pouring into a ball mill for mixing and grinding, and uniformly mixing and stirring the mixture with the prefabricated material in the step S1 after grinding to obtain mixed powder;
step S3, preparing a mixture
Weighing andalusite aggregate with the required mass percentage, adding the mixed powder in the step S2, adding water, and uniformly stirring to obtain a mixture;
step S4, casting and molding
Pouring the mixture in the step S3 into a mould to form a blank, and vibrating the mould to avoid generating bubbles inside the blank;
step S5, demolding and curing
Standing the die with the blank in the step S4 for 12-24 hours at normal temperature or constant temperature, taking out the die after the blank is molded, and naturally curing for 12-24 hours;
step S6, high-temperature calcination
And (5) putting the green body subjected to demoulding and curing in the step (S5) into a high-temperature kiln for calcination, and obtaining the tin bath top cover brick after calcination.
Further, in step S5, the conditions of the calcination are as follows: heating the blank to 150 ℃ within 48 hours, wherein the heating rate is 2.2-3.2 ℃/h; after keeping the temperature at 150 ℃ for 24 hours, heating the blank to 600 ℃ within 48-72 hours, wherein the heating rate is 17.5-19.5 ℃/h; after keeping the temperature at 600 ℃ for 24 hours, heating the blank to 1400 ℃ within 24-36 hours, wherein the heating rate is 25-35 ℃/h; after the temperature is kept at 1400 ℃ for 12 hours, the green body is gradually cooled to 100 ℃ within 24-48 hours, and the green body is calcined and discharged from the kiln, wherein the cooling rate is 45-55 ℃/h.
Further, in step S5, the temperature of the natural curing is 10-35 ℃.
Further, in the step S3, the mass of the added water accounts for 5-10% of the total mass of the raw material components;
in the step S4, the mode of vibrating the die comprises manual vibration or mechanical vibration, the vibration time is less than or equal to 25 minutes, and the vibration frequency is 125-250 times/minute.
The technical scheme of the application has the following beneficial effects:
(1) According to the tin bath top cover brick for float glass production, the raw material components are combined, and the corresponding mass ratio is combined, so that the prepared top cover brick has the advantages of small heat conductivity coefficient, high strength, light weight, good thermal shock resistance, good corrosion resistance and the like, and further the production quality of glass is conveniently improved.
(2) According to the preparation method of the tin bath top cover brick for float glass production, the low-scale high-temperature composite phase powder formed by the combination of andalusite fine powder and sol and the calcination pretreatment is adopted in the raw material components, wherein mineral phases such as mullite, quartz and undegraded andalusite exist, and the like, and the mineral phases still have the capacities of expanding, decomposing and reacting with other mineral phases like andalusite particles in the use process, and the generation and crack expansion of new cracks can be prevented through the process and the control of the mineral phases, so that the thermal shock resistance of a finished product is improved, and the phenomena of cracking and glass phase dripping are reduced;
by using the sol in the raw material components, gaps generated by cracks of the top cover bricks are effectively filled in the calcination process, so that the compactness of the top cover bricks is improved, the erosion gas is prevented from entering the top cover bricks, the deep corrosion of the erosion gas to the top cover bricks is restrained, the strength of the top cover bricks is improved, and the service life is prolonged; furthermore, the heat conductivity of the tin bath top cover brick can be reduced;
by using the glass phase forming agent in the raw material components, the top cover brick can react with silica powder raw materials or andalusite aggregate decomposed product formed by silica and the like at about 1000 ℃ to form a glass phase with higher viscosity, so that not only can the air holes on the inner surface of the top cover brick be sealed to prevent gas from escaping, but also the formed glass phase has higher viscosity and is not easy to drip, and meanwhile, the glass phase can fill grain gaps and bonding grains in the top cover brick, so that the surface of the top cover brick is denser, and when the compactness of the surface of the material is increased, the anti-seepage and slag resistance of the top cover brick can be correspondingly improved, thereby ensuring that the top cover brick has good heat preservation and gas seepage resistance;
the application greatly improves the heat stability, corrosion resistance and thermal shock resistance of the tin bath top cover brick by utilizing the synergistic effect of the raw material components, and simultaneously can reduce the heat conductivity of the tin bath top cover brick. In addition, the roof brick prepared by the application can also be directly piled up for use, thereby greatly reducing the weight of the tin bath roof and facilitating construction.
(3) According to the preparation method of the tin bath top cover brick for float glass production, through the step S1, the andalusite fine powder and sol are subjected to primary treatment, and a prefabricated material which is compact and has complex mineral phase components is obtained; through the step S2, various fine powder raw materials are mixed to be in uniform contact with each other, so that the quality of the finally obtained top cover brick is ensured to be stable; step S3, obtaining a mixture; step S4, obtaining a blank of the top cover brick; through the step S5, the raw materials are interacted and adhered and formed through natural curing; through the step S6, the mineral composition of the raw materials can be selectively changed and the crystal form transformation can be generated, so that the strength of the roof brick can be improved; through the combined use of the steps S1-S6, the roof brick with low heat conductivity and strong thermal shock resistance can be obtained. The preparation method is simple in process, low in cost, easy to realize industrial production, and good in performance of the prepared top cover brick, and suitable for popularization and application production.
Detailed Description
The following description of the embodiments of the present application will clearly and fully describe the technical aspects of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the application, fall within the scope of protection of the application.
Example 1:
the tin bath top cover brick for float glass production comprises the following raw material components in percentage by mass: 70% of andalusite aggregate, 12% of andalusite fine powder, 6% of pure calcium aluminate cement, 5% of alumina micropowder, 4% of sol, 1.8% of silica micropowder, 0.9% of glass phase forming agent and 0.3% of water reducer.
The andalusite aggregate and the andalusite fine powder comprise the following components in percentage by mass: al (Al) 2 O 3 60-65% of Fe 2 O 3 0.1 to 0.3 mass percent of Na 2 O, mgO and K 2 The sum of the mass percentages of O is less than or equal to 0.5 percent, wherein Na 2 O is 0.05 percent by mass, mgO is 0.05 percent by mass, K is the same as the weight percentage of the magnesium alloy 2 The mass percentage of O is 0.05%.
The sol is silica sol.
The glass phase forming agent is albite.
The pure calcium aluminate cement comprises the following components in percentage by mass: al (Al) 2 O 3 75% by mass and 25% by mass of CaO;
the alumina micropowder is alpha-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein, the mass percent is alpha-Al 2 O 3 The purity of (2) is 99.9%;
in the silicon micropowder, siO 2 The mass percentage of (2) is 95%;
the water reducing agent is sodium tripolyphosphate.
The grain size of andalusite aggregate is less than or equal to 5mm; the grain size of the andalusite fine powder is 200-325 meshes; the granularity of the pure calcium aluminate cement is not more than 300 meshes; the grain diameter of the alumina micropowder is 2-4 mu m; the particle size of the silicon micropowder is 0.3-2 μm.
The preparation method of the tin bath top cover brick for float glass production comprises the following steps:
step S1, preparing a prefabricated material
Weighing andalusite fine powder and sol with required mass percentages, stirring and uniformly mixing, putting into a muffle furnace, heating to 1400 ℃, preserving heat for 2 hours, stopping heating, cooling to room temperature, taking out, putting into a ball mill, and grinding until the particle size is 10-20 microns, thereby preparing a prefabricated material;
s2, preparing mixed powder
Weighing the pure calcium aluminate cement, the alumina micropowder, the silica micropowder, the water reducer and the glass phase forming agent which are in the required mass percentage, sequentially pouring the materials into a ball mill for mixing and grinding until the particle sizes of the raw materials are consistent and the raw materials are uniformly mixed, and uniformly mixing the raw materials with the prefabricated materials in the step S1 to obtain mixed powder;
step S3, preparing a mixture
And (2) weighing andalusite aggregate with the required mass percentage, adding the mixed powder in the step (S2), adding water, and uniformly stirring to obtain a mixture.
Step S4, casting and molding
Pouring the mixture obtained in the step S3 into a mould to form a blank body, and vibrating the mould to avoid generating bubbles inside the blank body;
step S5, demolding and curing
Standing the die with the blank in the step S4 for 18 hours at normal temperature, taking out the die after the blank is molded, and naturally curing for 15 hours;
step S6, high-temperature calcination
And (5) putting the green body subjected to demoulding and curing in the step (S5) into a high-temperature kiln for calcination, and obtaining the tin bath top cover brick after calcination.
In step S6, the conditions of the calcination are as follows: heating the blank to 150 ℃ within 48 hours, wherein the heating rate is 2.5-3.0 ℃/h; after keeping the temperature at 150 ℃ for 24 hours, heating the blank to 600 ℃ within 48-72 hours, wherein the heating rate is 18-19 ℃/h; after keeping the temperature at 600 ℃ for 24 hours, heating the blank to 1400 ℃ within 24-36 hours, wherein the heating rate is 28-30 ℃/h; after the temperature is kept at 1400 ℃ for 12 hours, the green body is gradually cooled to 100 ℃ within 24-48 hours, and the green body is calcined and discharged from the kiln, wherein the cooling rate is 48-50 ℃/h.
In step S5, the temperature of the natural curing is 20 ℃.
In the step S3, the mass of the added water accounts for 8% of the total mass of the raw material components;
in step S4, the mode of vibrating the mold includes manual vibration or mechanical vibration, the vibration time is 20 minutes, and the vibration frequency is 125 times per minute.
Examples 2 to 5 and comparative examples 1 to 6 were also made according to the present application, except that examples 2 to 5 were different only in the amounts of the respective raw material components, the specific amounts being shown in Table 1, and Table 1 also shows the performance data of the ordinary commercially available tin bath ceiling tile (ordinary commercially available tin bath ceiling tile is a tin bath ceiling tile of the New country Jiang Xin refractory Co., ltd.) and the tin bath ceiling tiles produced from examples 1 to 5 and comparative examples 1 to 6. The data in Table 1 are obtained by measuring the thermal shock resistance of the GB/T30873-2014 refractory material.
TABLE 1
Table 1, below
As can be seen from the data in table 1, the volume density of the float glass tin bath roof bricks with thermal shock resistance obtained in examples 1 to 5 is smaller than that of the common commercial tin bath roof bricks, the porosity is larger than that of the common commercial tin bath roof bricks, and the float glass tin bath roof bricks are not easy to crack and slag; the heat conductivity coefficient is smaller than that of common tin bath top cover bricks and has good thermal shock resistance. Experimental results show that the float glass tin bath top cover brick prepared by the application has high temperature resistance and strong thermal shock resistance compared with common tin bath top cover bricks sold in the market.
The use of too high or too low an amount of andalusite fine powder in comparative examples 1-2 resulted in a decrease in the thermal shock resistance of the resulting tin bath ceiling tile as compared to examples 1-5.
Comparative examples 3-4, either without the use of a glass phase former or with an excessively high amount of a glass phase former, resulted in a decrease in thermal shock resistance of the resulting tin bath ceiling tile, while an increase in thermal conductivity resulted in an increase in thermal conductivity.
Comparative examples 5 to 6, compared to examples 1 to 5, use of neither sol nor an excessively high amount of sol resulted in a decrease in thermal shock resistance and refractoriness of the resulting tin bath ceiling tile, while an increase in thermal conductivity resulted in an increase in thermal conductivity.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (7)
1. The preparation method of the tin bath top cover brick for producing the float glass is characterized by comprising the following raw material components in percentage by mass: 60% -74% of andalusite aggregate, 10% -15% of andalusite fine powder, 4% -9% of pure calcium aluminate cement, 3% -9% of alumina micropowder, 3% -8% of sol, 0.1% -5% of silica micropowder, 0.1% -3% of glass phase forming agent and 0.1% -0.5% of water reducer;
the andalusite aggregate and the andalusite fine powder comprise the following components in percentage by mass: al (Al) 2 O 3 The mass percentage of (2) is more than or equal to 58 percent, fe 2 O 3 Is less than or equal to 0.5 percent of Na by mass 2 O, mgO and K 2 The sum of the mass percentages of O is less than or equal to 0.5 percent
The preparation method of the tin bath top cover brick for float glass production comprises the following steps:
step S1, preparing a prefabricated material
Weighing andalusite fine powder and sol with required mass percentages, stirring and uniformly mixing, heating to about 1200-1600 ℃, preserving heat for 1-4 hours, stopping heating, cooling to room temperature, taking out, and placing in a ball mill for grinding until the particle size is 5-25 microns, thereby preparing a prefabricated material;
s2, preparing mixed powder
Weighing the pure calcium aluminate cement, the alumina micropowder, the silica micropowder, the water reducer and the glass phase forming agent which are in the required mass percentage, pouring into a ball mill for mixing and grinding, and uniformly mixing and stirring the mixture with the prefabricated material in the step S1 after grinding to obtain mixed powder;
step S3, preparing a mixture
Weighing andalusite aggregate with the required mass percentage, adding the mixed powder in the step S2, adding water, and uniformly stirring to obtain a mixture;
step S4, casting and molding
Pouring the mixture into a mould to form a blank body, and vibrating the mould to avoid bubbles in the blank body;
step S5, demolding and curing
Standing the die with the blank in the step S4 for 12-24 hours at normal temperature or constant temperature, taking out the die after the blank is molded, and naturally curing for 12-24 hours;
step S6, high-temperature calcination
Placing the green body subjected to demoulding and curing in the step S5 into a high-temperature kiln for calcination to obtain a tin bath top cover brick;
in step S6, the conditions of the calcination are as follows: heating the blank to 150 ℃ within 48 hours, wherein the heating rate is 2.2-3.2 ℃/h; after keeping the temperature at 150 ℃ for 24 hours, heating the blank to 600 ℃ within 48-72 hours, wherein the heating rate is 17.5-19.5 ℃/h; after keeping the temperature at 600 ℃ for 24 hours, heating the blank to 1400 ℃ within 24-36 hours, wherein the heating rate is 25-35 ℃/h; after the temperature is kept at 1400 ℃ for 12 hours, the green body is gradually cooled to 100 ℃ within 24-48 hours, and the green body is calcined and discharged from the kiln, wherein the cooling rate is 45-55 ℃/h.
2. The method for producing a roof tile for a molten tin bath according to claim 1, wherein the sol is at least one of silica sol, alumina sol and silica-alumina sol.
3. The method of producing a tin bath roof brick for float glass production according to claim 1, wherein the glass phase forming agent comprises at least one of spodumene, albite and a mixture of potassium-sodium containing minerals.
4. The method for preparing a tin bath roof brick for float glass production according to claim 1, wherein the pure calcium aluminate cement comprises the following components in percentage by mass: al (Al) 2 O 3 70-80% by mass and 20-30% by mass of CaO;
the alumina micropowder is alpha-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein, the mass percent is alpha-Al 2 O 3 The purity of (2) is more than 99%;
in the silicon micropowder, siO 2 The mass percentage content of (2) is more than or equal to 95 percent;
the water reducer comprises at least one of sodium tripolyphosphate, sodium polyacrylate and sodium hexametaphosphate.
5. The method for producing a tin bath roof brick for float glass production according to claim 1, wherein the andalusite aggregate has a particle size of 5mm or less; the grain size of the andalusite fine powder is 200-325 meshes; the granularity of the pure calcium aluminate cement is not more than 300 meshes; the grain diameter of the alumina micropowder is 2-5 mu m; the particle size of the silicon micropowder is 0.3-2 μm.
6. The method for producing a tin bath roof brick for float glass production according to claim 1, wherein in step S5, the natural curing temperature is 10 to 35 ℃.
7. The method for producing a tin bath top cover brick for float glass production according to claim 1, wherein in step S3, the mass of added water is 5% -10% of the total mass of the raw material components;
in the step S4, the mode of vibrating the die comprises manual vibration or mechanical vibration, the vibration time is less than or equal to 25 minutes, and the vibration frequency is 125-250 times/minute.
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Citations (5)
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US5846891A (en) * | 1997-06-10 | 1998-12-08 | Korea Institute Of Science And Technology | Thermal shock-resistant alumina-mullite composite material and preparation method thereof |
CN104086197A (en) * | 2014-07-12 | 2014-10-08 | 瑞泰科技股份有限公司 | Andalusite and cordierite refractory material for glass kiln and product thereof |
CN104086198A (en) * | 2014-07-12 | 2014-10-08 | 瑞泰科技股份有限公司 | Refractory andalusite material for glass kiln and product of refractory andalusite material |
JP2022026926A (en) * | 2020-07-31 | 2022-02-10 | Jfeスチール株式会社 | Monolithic refractory |
WO2022144014A1 (en) * | 2020-12-31 | 2022-07-07 | 郑州轻工业大学 | Mullite-based micro-nano-porous heat insulating refractory material and preparation method therefor |
Family Cites Families (1)
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JP4470207B2 (en) * | 2005-11-25 | 2010-06-02 | 品川リフラクトリーズ株式会社 | Refractory brick |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US5846891A (en) * | 1997-06-10 | 1998-12-08 | Korea Institute Of Science And Technology | Thermal shock-resistant alumina-mullite composite material and preparation method thereof |
CN104086197A (en) * | 2014-07-12 | 2014-10-08 | 瑞泰科技股份有限公司 | Andalusite and cordierite refractory material for glass kiln and product thereof |
CN104086198A (en) * | 2014-07-12 | 2014-10-08 | 瑞泰科技股份有限公司 | Refractory andalusite material for glass kiln and product of refractory andalusite material |
JP2022026926A (en) * | 2020-07-31 | 2022-02-10 | Jfeスチール株式会社 | Monolithic refractory |
WO2022144014A1 (en) * | 2020-12-31 | 2022-07-07 | 郑州轻工业大学 | Mullite-based micro-nano-porous heat insulating refractory material and preparation method therefor |
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