Large-size tin bath bottom brick and preparation method thereof

By optimizing the material composition and process flow of large-size tin bath bottom bricks through the preparation method, the problem of tin bath bottom bricks being easily damaged at high temperatures was solved, and the stable operation of the tin bath and the reduction of tin liquid penetration were achieved.

CN120717801APending Publication Date: 2025-09-30SHANDONG ZIBO SHENZI REFRACTORY MATERIALS CO LTD
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Patent Information

Application Number
CN202510984741.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-17
Publication Date
2025-09-30

AI Technical Summary

Technical Problem

Existing large-sized tin bath bottom bricks are easily damaged by chemical corrosion at high temperatures, have low compressive strength, are prone to expansion and fracture, and have a large amount of tin liquid penetration, leading to frequent production accidents.

Method used

Large-sized tin bath bottom bricks are prepared by using a combination of M70 mullite aggregate, andalusite homogenizer, calcium aluminate cement, activated alumina powder, zirconium composite silicon powder, α-A12O3 powder, Guangxi white mud, binders and additives through ball milling, mixing, vibration molding, curing, drying and high-temperature sintering.

Benefits of technology

The strength and thermal shock resistance of the tin bath bottom bricks are improved, the penetration of tin liquid is reduced, the loss of tin liquid is reduced, production accidents are avoided, and the stable operation of the tin bath is ensured.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a large-size tin bath bottom brick and a preparation method thereof, and the large-size tin bath bottom brick is prepared from the following raw materials in percentage by weight: 35% of M70 mullite aggregate, 45% of andalusite homogenized material, 1.5% of calcium aluminate cement, 5% of activated aluminum oxide micro powder, 3% of zirconium composite silicon micro powder, 5% of alpha-Al2O3 micro powder, 2.5% of Guangxi white mud, 0.5% of binding agent and 2.5% of additive. Compared with a traditional tin bath bottom brick, the prepared brick material is larger in size, the number of tin bath holes in the whole tin bath bottom is reduced by 20%, gaps between the tin bath bricks are reduced by 30%, the tin liquid permeation amount and the tin liquid loss cost are reduced, the tin liquid buoyancy is increased after the volume is increased, and therefore production accidents caused by breaking away from fixing bolts at the bath bottom are avoided; meanwhile, balanced expansion of the brick bodies is stabilized, the problems of expansion fracture after high temperature and scratching of the lower surface of the glass plate due to floating of edge fragments collapsed after expansion of the brick bodies in tin liquor are solved, and the good practicability is achieved.
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Description

Technical Field

[0001] The invention relates to the technical field of tin bath bottom brick production, in particular to a large-size tin bath bottom brick and a preparation method thereof. Background Art

[0002] Tin bath bricks are the key refractory materials for the tin bath in float glass production lines. They are in direct contact with high-temperature molten tin (approximately 600-1100°C) and must have the following characteristics: High density: prevents tin liquid penetration. Low porosity: reduces tin vapor corrosion. Chemical stability: resists corrosion from tin liquid and reducing atmospheres. Thermal shock resistance: adapts to temperature fluctuations.

[0003] The large-sized tin bath bottom bricks in the prior art are easily damaged by chemical erosion during actual use, have low compressive strength at high temperatures, and are easily expanded and fractured by high temperatures, which is inconvenient during use. Therefore, we propose a large-sized tin bath bottom brick and a preparation method thereof to solve the above problems. Summary of the Invention

[0004] Based on the technical problems existing in the background technology, the present invention proposes a large-sized tin bath bottom brick and a preparation method thereof.

[0005] The invention provides a large-size tin bath bottom brick comprising the following raw materials: 35% of M70 mullite aggregate, 45% of andalusite homogenizer, 1.5% of calcium aluminate cement, 5% of activated alumina fine powder, 3% of zirconium composite silicon fine powder, 5% of α-A12O3 fine powder, 2.5% of Guangxi white mud, 0.5% of a binder, and 2.5% of an additive.

[0006] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0007] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon powder, titanium dioxide and active α-Al2O3 powder.

[0008] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 35-45% of M70 mullite aggregate, 35-45% of andalusite homogenizer, 1.5-3.5% of calcium aluminate cement, 3-5% of activated alumina powder, 3-5% of zirconium composite silicon powder, 6-10% of α-A12O3 powder, 1-2.5% of Guangxi white mud, 0.5% of binder and 1-4% of additives; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 3-8% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibration rod into the robot arm to remove bubbles, and vibrate at high frequency for 5-10 minutes; S5: Allow the vibrated mixture to stand for 24-36 hours and then demold and cure for 12-15 hours; S6: Send the cured rough bricks into the drying room and dry them for 50-70 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0009] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0010] Preferably, in the step S4, the vibration frequency of the vibration platform is 150-300 times / second, the mixing time of the mixture is 5-10 minutes, and the trapped time is 5-10 minutes.

[0011] Preferably, in step S6, the drying temperature is 40-60°C.

[0012] Preferably, the embryo body calcination temperature in step S7 is 600-1500°C.

[0013] The bricks prepared by the present invention are larger in size than traditional tin bath bottom bricks, reduce the number of tin bath holes on the entire tin bath bottom by 20%, reduce the gaps between tin bath bricks by 30%, reduce the amount of tin liquid penetration and the cost of tin liquid loss, and resist the increase in buoyancy of the tin liquid due to the increase in volume, thereby avoiding production accidents caused by escaping from the fixing bolts at the bottom of the bath. At the same time, the bricks stabilize the balanced expansion, avoid expansion fracture after high temperature, and avoid the problem of edge fragments between bricks collapsing after expansion floating in the tin liquid and scratching the lower surface of the glass plate, and have good practicality. DETAILED DESCRIPTION

[0014] The present invention will be further explained below with reference to specific embodiments.

[0015] Example 1 This embodiment provides a large-sized tin bath bottom brick, comprising the following raw materials: 35% M70 mullite aggregate, 45% andalusite homogenizer, 1.5% calcium aluminate cement, 5% activated alumina powder, 3% zirconium composite silicon powder, 5% α-Al2O3 powder, 2.5% Guangxi white mud, 0.5% binder, and 1% additive.

[0016] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0017] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon micropowder, titanium dioxide and active α-AL2O3 micropowder.

[0018] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 38% of M70 mullite aggregate, 35% of andalusite homogenizer, 2% of calcium aluminate cement, 5% of activated alumina powder, 5% of zirconium composite silicon powder, 8% of α-Al2O3 powder, 2.5% of Guangxi white mud, 0.5% of binder and 1% of additives; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 3% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibrating rod into the robot arm to remove bubbles, and vibrate at high frequency for 10 minutes; S5: Curing the vibrated mixture for 26 hours and then demolding and curing for 15 hours; S6: Send the cured rough bricks into the drying room and dry them for 70 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0019] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0020] Preferably, in the step S4, the vibration frequency of the vibration platform is 180 times / second, the mixing time of the mixture is 8 minutes, and the trapped time is 10 minutes.

[0021] Preferably, in step S6, the drying temperature is 50°C.

[0022] Preferably, the embryo body calcination temperature in step S7 is 1200°C.

[0023] Example 2 This embodiment provides a large-sized tin bath bottom brick, comprising the following raw materials: 39% M70 mullite aggregate, 35% andalusite homogenizer, 2% calcium aluminate cement, 3% activated alumina powder, 4% zirconium composite silicon powder, 8% α-A12O3 powder, 2.5% Guangxi white mud, 0.5% binder, and 1% additive.

[0024] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0025] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon micropowder, titanium dioxide and active α-A12O3 micropowder.

[0026] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 39% of M70 mullite aggregate, 35% of andalusite homogenizer, 2% of calcium aluminate cement, 3% of activated alumina powder, 4% of zirconium composite silicon powder, 8% of α-A12O3 powder, 2.5% of Guangxi white mud, 0.5% of binder and 1% of additives; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 5% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibration rod into the robot arm to remove bubbles, and vibrate at high frequency for 80 minutes; S5: Curing the vibrated mixture for 36 hours and then demolding and curing for 12 hours; S6: Send the cured rough bricks into the drying room and dry them for 50 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0027] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0028] Preferably, in the step S4, the vibration frequency of the vibration platform is 200 times / second, the mixing time of the mixture is 10 minutes, and the trapped time is 10 minutes.

[0029] Preferably, in step S6, the drying temperature is 60°C.

[0030] Preferably, the embryo body calcination temperature in step S7 is 900°C.

[0031] Example 3 This embodiment provides a large-sized tin bath bottom brick, comprising the following raw materials: 39% M70 mullite aggregate, 39% andalusite homogenizer, 1.5% calcium aluminate cement, 3% activated alumina powder, 3% zirconium composite silicon powder, 6% α-Al2O3 powder, 1% Guangxi white mud, 0.5% binder, and 2.5% additives.

[0032] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0033] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon micropowder, titanium dioxide and active α-AL2O3 micropowder.

[0034] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 39% of M70 mullite aggregate, 39% of andalusite homogenizer, 1.5% of calcium aluminate cement, 3% of activated alumina powder, 3% of zirconium composite silicon powder, 6% of α-AL2O3 powder, 1% of Guangxi white mud, 0.5% of binder and 2.5% of additives according to the parts; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 4.5% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibrating rod into the robot arm to remove bubbles, and vibrate at high frequency for 10 minutes; S5: Curing the vibrated mixture for 36 hours and then demolding and curing for 15 hours; S6: Send the cured rough bricks into the drying room and dry them for 50 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0035] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0036] Preferably, in the step S4, the vibration frequency of the vibration platform is 300 times / second, the mixing time of the mixture is 5 minutes, and the trapped time is 5 minutes.

[0037] Preferably, in step S6, the drying temperature is 40°C.

[0038] Preferably, the embryo body calcination temperature in step S7 is 1350°C.

[0039] Example 4 This embodiment provides a large-sized tin bath bottom brick, comprising the following raw materials: 40% M70 mullite aggregate, 35% andalusite homogenizer, 2% calcium aluminate cement, 3% activated alumina powder, 4% zirconium composite silicon powder, 6% α-Al2O3 powder, 2.5% Guangxi white mud, 0.5% binder, and 2.5% additives.

[0040] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0041] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon micropowder, titanium dioxide and active α-AL2O3 micropowder.

[0042] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 40% of M70 mullite aggregate, 35% of andalusite homogenizer, 2% of calcium aluminate cement, 3% of activated alumina powder, 4% of zirconium composite silicon powder, 6% of α-AL2O3 powder, 2.5% of Guangxi white mud, 0.5% of binder and 2.5% of additives; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 4.5% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibrating rod into the robot arm to remove bubbles, and vibrate at high frequency for 10 minutes; S5: Curing the vibrated mixture for 30 hours and then demolding and curing for 145 hours; S6: Send the cured rough bricks into the drying room and dry them for 65 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0043] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0044] Preferably, in the step S4, the vibration frequency of the vibration platform is 300 times / second, the mixing time of the mixture is 10 minutes, and the trapped time is 10 minutes.

[0045] Preferably, in step S6, the drying temperature is 55°C.

[0046] Preferably, the embryo body calcination temperature in step S7 is 760°C.

[0047] Example 5 This embodiment provides a large-sized tin bath bottom brick, comprising the following raw materials: 42% M70 mullite aggregate, 35% andalusite homogenizer, 1.5% calcium aluminate cement, 3.5% activated alumina powder, 3% zirconium composite silicon powder, 6% α-Al2O3 powder, 1% Guangxi white mud, 0.5% binder, and 2.5% additives.

[0048] Preferably, the binder is one or more of phosphoric acid, pulp, starch, polyvinyl alcohol, boron oxide, aluminate cement and calcium aluminate cement.

[0049] Preferably, the additive is one or more of sodium hydroxymethyl cellulose, water reducing agent, silicon micropowder, titanium dioxide and active α-AL2O3 micropowder.

[0050] The present invention also provides a method for preparing large-sized tin bath bottom bricks, comprising the following steps: S1: Weigh 42% of M70 mullite aggregate, 35% of andalusite homogenizer, 1.5% of calcium aluminate cement, 3.5% of activated alumina powder, 3% of zirconium composite silicon powder, 6% of α-AL2O3 powder, 1% of Guangxi white mud, 0.5% of binder and 2.5% of additives according to the number of parts; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 5% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibrating rod into the robot arm to remove bubbles, and vibrate at high frequency for 6 minutes; S5: Curing the vibrated mixture for 28 hours and then demolding and curing for 12 hours; S6: Send the cured rough bricks into the drying room and dry them for 70 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

[0051] Preferably, in step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

[0052] Preferably, in the step S4, the vibration frequency of the vibration platform is 250 times / second, the mixing time of the mixture is 8 minutes, and the trapped time is 6 minutes.

[0053] Preferably, in step S6, the drying temperature is 50°C.

[0054] Preferably, the embryo body calcination temperature in step S7 is 1150°C.

[0055] Compared with conventional tin bath bottom bricks (parameters of conventional tin bath bottom bricks: AL2O3 (%): 43±2, Fe2O3 (%) ≤1.2, bulk density (g / cm 3 ) ≥ 2.2, apparent porosity % ≤ 20 and normal temperature pressure resistance (MPa) ≥ 40), the tin bath bottom bricks prepared by Examples 1 to 5 are as follows: Table 1:

[0056] Table 2:

[0057] As can be seen from Table 1 and Table 2 above, the tin bath bottom bricks proposed in the present invention improve the brick body strength, pressure resistance, strength, apparent porosity, thermal conductivity and room temperature pressure resistance index.

[0058] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A large-size tin bath bottom brick, characterized in that: The raw materials include the following proportions: 35% M70 mullite aggregate, 45% andalusite homogenizer, 1.5% calcium aluminate cement, 5% activated alumina micropowder, 3% zirconium composite silicon micropowder, 5% α-A12O3 micropowder, 2.5% Guangxi white mud, 0.5% binder and 2.5% additives.

2. A large-size tin bath bottom brick according to claim 1, characterized in that: The binder is one or more of pulp, starch, polyvinyl alcohol, boron oxide and aluminate cement.

3. The large-size tin bath bottom brick according to claim 1, characterized in that: The additive is one or more of sodium hydroxymethyl cellulose, titanium dioxide and active α-A1 micropowder.

4. The method for preparing a large-size tin bath bottom brick according to claim 1, characterized in that: The following steps are involved: S1: Weigh 35-45% of M70 mullite aggregate, 35-45% of andalusite homogenizer, 1.5-3.5% of calcium aluminate cement, 3-5% of activated alumina powder, 3-5% of zirconium composite silicon powder, 6-10% of α-A12O3 powder, 1-2.5% of Guangxi white mud, 0.5% of binder and 1-4% of additives; S2: Add the homogenized andalusite material into the ball mill and grade the particles according to different particle requirements, grind and sieve to obtain fine powder; S3: Add 3-8% water to the above raw materials weighed in portions and mix to obtain a mixture; S4: Pour the mixture into a steel mold, place the steel mold flat on a vibration platform, insert a vibration rod into the robot arm to remove bubbles, and vibrate at high frequency for 5-10 minutes; S5: Allow the vibrated mixture to stand for 24-36 hours and then demold and cure for 12-15 hours; S6: Send the cured rough bricks into the drying room and dry them for 50-70 hours; S7: The dried rough bricks are placed in a high-temperature shuttle kiln and sintered for 30 days; S8: After cooling out of the kiln, according to the requirements of the drawing, precise drilling, six-sided cutting and polishing are carried out to ensure that the tolerance size is controlled between 0-1mm.

5. The method for preparing a large-sized tin bath bottom brick according to claim 4, characterized in that: In the step S1, the average particle size of the M70 mullite aggregate is ≤10 mm polygonal particles, the andalusite homogenized material can be graded as 20%≤5 mm, 20%≤3 mm, 10%≤1 mm, 30%≤800 mesh, 20%≤300 mesh, and the average particle size of Guangxi white mud is ≤4.3 μm.

6. The method for preparing a large-sized tin bath bottom brick according to claim 4, characterized in that: In the step S4, the vibration frequency of the vibration platform is 150-300 times / second, the mixing time of the mixture is 5-10 minutes, and the material trapping time is 5-10 minutes.

7. The method for preparing a large-sized tin bath bottom brick according to claim 4, characterized in that: In step S6, the drying temperature is 40-60°C.

8. The method for preparing a large-sized tin bath bottom brick according to claim 4, characterized in that: In the step S7, the embryo body is calcined at a temperature of 600-1500°C.