CN102557688B - Preparation method for isostatic pressure calcium-aluminum-silicon tin bath bottom brick - Google Patents

Preparation method for isostatic pressure calcium-aluminum-silicon tin bath bottom brick Download PDF

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CN102557688B
CN102557688B CN2012100027185A CN201210002718A CN102557688B CN 102557688 B CN102557688 B CN 102557688B CN 2012100027185 A CN2012100027185 A CN 2012100027185A CN 201210002718 A CN201210002718 A CN 201210002718A CN 102557688 B CN102557688 B CN 102557688B
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tin bath
bottom brick
molten tin
calcium
preparation
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CN102557688A (en
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张启山
张瑛
车建壮
李志军
孙文礼
刘杰
冯延春
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Zibo Gongtao New Materials Group Co., Ltd.
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ZIBO INDUSTRIAL CERAMIC REFRACTORY MATERIAL Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • C03—GLASS; MINERAL OR SLAG WOOL
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Abstract

The invention relates to a tin bath bottom brick and a preparation method thereof and belongs to the technical field of refractory materials. The tin bath bottom brick comprises the following chemical components in percentage by mass: 67 to 76 percent of Al2O3, 21 to 28 percent of CaO, 1.5 to 5 percent of SiO2 and the balance of common ore impurities. The tin bath bottom brick is prepared by preparing materials, performing isostatic pressure formation and sintering at high temperature, wherein the materials comprise the following components in percentage by weight: 30 to 45 percent of calcium aluminate coarse particles with the particle size of 3 to 1mm, 20 to 35 percent of calcium aluminate medium particles with the particle size of 1 to 0.1 mm and 25 to 40 percent of combined powder with the particle size of less than 0.088 mm. The product has high alkali metal oxide corrosion resistance, low thermal expansion rate, low thermal conductivity and low hydrogen diffusion rate.

Description

Preparation method Deng the siliceous bottom brick of molten tin bath of static pressure aluminium calcium
Technical field
The present invention relates to a kind of bottom brick of molten tin bath and method for making thereof, belong to technical field of refractory materials.
Technical background
Molten tin bath is the key equipment of float flat glass production line, and the glass metal after the fusing flows in the molten tin bath, swims on the tin liquor, forms level and smooth plate glass when advancing, and stores the used refractory brick of tin liquor and is called bottom brick of molten tin bath.The majority that uses in the market is the sal clay brick, in its use, because contained Na2O infiltrates in the brick lentamente through tin liquor in the glass, forms nepheline and also produces volumetric expansion and thermal stresses.When the metamorphic layer that contains nepheline was increased to certain thickness, metamorphic layer can peel off in the form of sheets, because its proportion is lower than tin liquor, when the fragment that peels off floats on the tin liquor face, can cause glass surface to scratch and glass defect.
The researchist of magnesium company (RHI) difficult to understand has adopted the basic material calcium aluminate to make bottom brick of molten tin bath, as described in patent US5420087, the said firm is raw material with calcium aluminate coarse particles and fine particle, and the employing calcium aluminate is binding agent, through vibratory compaction, dry after the maintenance, burn till.It is characterized in that adopting the calcium aluminate coarse particles of porous and fine particle is raw material, aquation keying action with calcium aluminate forms the brick body, making 1100 ℃ of burning posterior spiracle rates is 43%, alkali resistance oxide erosion, the calcium aluminate bottom brick of molten tin bath that coefficient of thermal expansion is low, thermal conductivity is low, gas permeation rate is low.Point out in the patent: for prevent brick in use with alkalimetal oxide reaction and reducing atmosphere under other reactions, SiO in the raw material 2, Fe 2O 3Mass percentage content should be lower than 1.5%, SiO respectively 2, Fe 2O 3Content preferably only be a small amount of.The shortcoming of this brick is that coarse particles is combined by hydrate between fine particle, and after 1100 ℃ of thermal treatments, calcium aluminate still comprises on a small quantity in conjunction with water in mutually, in temperature use more than 1100 ℃, also will overflow in conjunction with water, the void content of goods also can increase, and can cause application risk.
Summary of the invention
The object of the present invention is to provide a kind of siliceous bottom brick of molten tin bath of aluminium calcium of high temperature sintering, alkaline-resisting metal oxide aggressiveness is good, coefficient of thermal expansion is low, thermal conductivity is low, the hydrogen diffusivity is low.
The present invention provides its preparation method who rationally easily goes simultaneously.
The siliceous bottom brick of molten tin bath of aluminium calcium of the present invention, its chemical constitution mass percent is Al 2O 367-76%, CaO 21-28%, SiO 2Be 1.5-5%, surplus is common dirt, as MgO, Na 2O etc.
The XRD mineral facies of product consist of two calcium aluminates account for 70-90%, calcium hexaluminate and account for≤10% and gehlenite account for 8-25%.
The void content of product is 18-24%.
Rationally easily the preparation method of row is as follows:
After batching, moulding, high temperature burn till, make, it is characterized in that ingredients by weight per-cent is: particle diameter be particle 20-35% in the calcium aluminate coarse particles 30-45% of 3-1mm, the calcium aluminate that particle diameter is 1-0.1mm,＜0.088mm is in conjunction with fine powder 25-40%.
Wherein, the void content of calcium aluminate raw material is less than 3%, and its chemical constitution mass percent is: Al 2O 373-79%, CaO 21-27%, Fe 2O 3≤ 0.10%.
Be the mixture of calcium aluminate fine powder, alpha-alumina fine powder and silica compound fine powder in conjunction with fine powder, press SiO 2The 1.5-5% that accounts for compound chemical constitution mass percent adds the silica compound fine powder, presses SiO in the mixture 2The 0.8-1.4 of mass percent doubly adds alpha-aluminium oxide powder, and all the other are the calcium aluminate fine powder.
In conjunction with silica compound in the fine powder be select for use at least in clay, quartz, diopside, the wollastonite a kind of.
After batch mixes, adopt the moulding of isostatic pressing mode to get base substrate, forming pressure is 50-200Mpa.
Burn till behind the body drying, general nature was gone into klining in dry 1-3 days.
Firing temperature is 1300-1450 ℃, and burning till soaking time is 10-40 hour.
The firing temperature system is as follows:
10 ℃-200 ℃ heat-up rate 1-2 ℃/minute
200 ℃-1300 ℃ heat-up rate 1-3 ℃/minute
1300-1450 ℃ of insulation, soaking time are 10-40 hour
Cease fire and lower the temperature naturally cooling.
Compared with prior art, the present invention has following beneficial effect:
It is coarse particles and fine particle that the present invention adopts fine and close calcium aluminate, and adding alpha-aluminium oxide powder and silica compound powder is wedding agent, through isostatic pressing, to burn till back formation be the product of essential mineral phase with two calcium aluminates, gehlenite, calcium hexaluminate.Do not contain hydrate in the product, internal structure is even, anti-tin liquor good penetrability, alkaline-resisting metal oxide corrode, coefficient of thermal expansion is low, thermal conductivity is low, the hydrogen diffusivity is low, solve clay matter bottom brick of molten tin bath and be subject to alkalimetal oxide erosion generation nepheline, the problem that causes brick volumetric expansion, peeling, can improve the work-ing life of bottom brick of molten tin bath, and can reduce by the glass defect of bottom brick of molten tin bath generation and the calorific loss of molten tin bath bottom.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment
In the physical and chemical index such as following table 1 of raw materials such as calcium aluminate particles, alpha-aluminium oxide powder, silica compound powder, join raw material in the mixing roll in proportion, mix after 5-15 minute, in the inferior static pressure compression moulding of 50-200Mpa pressure, after base substrate seasoning 1-3 days, burn till at 1300 ℃-1450 ℃ and to make the siliceous bottom brick of molten tin bath sample of aluminium calcium, detect physical and chemical indexs such as its chemical ingredients, mineral facies composition, void content, volume density, compressive strength, thermal conductivity and see specific embodiment table 2.
The quality chemistry percentage composition table of table 1 raw material
Figure BDA0000129081440000031
Table 2, specific embodiment table
Figure BDA0000129081440000032
MgO, Na in the siliceous bottom brick of molten tin bath of * aluminium calcium 2Mineralogical compositions such as O form small amount of magnesium aluminate or glassy phase, so the essential mineral resultant less than 100% of two calcium aluminates, gehlenite, calcium hexaluminate mutually.

Claims (10)

1. the siliceous bottom brick of molten tin bath of aluminium calcium of an isostatic pressing is characterized in that the chemical constitution mass percent is Al 2O 367-76%, CaO 21-28%, SiO 2Be 1.5-5%, surplus is common dirt.
2. the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 1, the XRD mineral facies that it is characterized in that product consist of that two calcium aluminates account for 70-90%, gehlenite accounts for 8-25%.
3. the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 2, the XRD mineral facies that it is characterized in that product contain calcium hexaluminate≤10% in forming.
4. the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 1, the void content that it is characterized in that product is 18-24%.
5. the preparation method of the siliceous bottom brick of molten tin bath of the described aluminium calcium of claim 1, after batching, isostatic pressing, high temperature burn till, make, it is characterized in that ingredients by weight per-cent is: particle diameter be particle 20-35% in the calcium aluminate coarse particles 30-45% of 3-1mm, the calcium aluminate that particle diameter is 1-0.1mm,＜0.088mm is in conjunction with fine powder 25-40%.
6. the preparation method of the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 5 is characterized in that the void content of calcium aluminate raw material less than 3%, and its chemical constitution mass percent is: Al 2O 373-79%, CaO 21-27%, Fe 2O 3≤ 0.10%.
7. the preparation method of the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 5 is characterized in that in conjunction with fine powder being the mixture of calcium aluminate fine powder, alpha-alumina fine powder and silica compound fine powder, presses SiO 2The 1.5-5% that accounts for compound chemical constitution mass percent adds the silica compound fine powder, presses SiO in the mixture 2The 0.8-1.4 of mass percent doubly adds alpha-aluminium oxide powder, and all the other are the calcium aluminate fine powder.
8. the preparation method of the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 7, it is characterized in that in conjunction with silica compound in the fine powder be select for use at least in clay, quartz, diopside, the wollastonite a kind of.
9. the preparation method of the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 5 is characterized in that after the batch mixes, adopts the moulding of isostatic pressing mode to get base substrate, and forming pressure is 50-200Mpa.
10. the preparation method of the siliceous bottom brick of molten tin bath of aluminium calcium according to claim 5 is characterized in that burning till behind the body drying, and firing temperature is 1300-1450 ℃, and burning till soaking time is 10-40 hour.
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PCT/CN2012/001713 WO2013102288A1 (en) 2012-01-06 2012-12-21 Tin bath bottom brick of aluminium, calcium and silicon, and method for preparing same

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CN102557688B (en) * 2012-01-06 2013-08-14 淄博工陶耐火材料有限公司 Preparation method for isostatic pressure calcium-aluminum-silicon tin bath bottom brick
CN104909542B (en) * 2015-05-09 2017-09-22 浙江瑞泰耐火材料科技有限公司 A kind of bottom brick of molten tin bath
CN104914020A (en) * 2015-05-09 2015-09-16 浙江瑞泰耐火材料科技有限公司 Tin bath bottom brick hydrogen diffusion degree detection apparatus
CN106518043B (en) * 2016-11-17 2019-05-14 淄博工陶耐火材料有限公司 The preparation method of the siliceous bottom brick of molten tin bath of low-cost aluminum calcium
CN107892579B (en) * 2017-11-23 2020-10-09 淄博工陶新材料集团有限公司 Calcium aluminate glass kiln tin bath suspended ceiling brick and preparation method thereof
CN116751068B (en) * 2023-08-18 2023-10-31 山东淄博沈淄耐火材料有限公司 Method for preparing isostatic pressing forming calcium-tin aluminate bottom bricks

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