CN101830718B - Manufacturing method of corundum zircon brick - Google Patents

Manufacturing method of corundum zircon brick Download PDF

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CN101830718B
CN101830718B CN 201010171534 CN201010171534A CN101830718B CN 101830718 B CN101830718 B CN 101830718B CN 201010171534 CN201010171534 CN 201010171534 CN 201010171534 A CN201010171534 A CN 201010171534A CN 101830718 B CN101830718 B CN 101830718B
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corundum
weight parts
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zircon
brick
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张世俭
涂淑进
阮小川
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Guangzhou City Baiyun District Shijing Refractory Material Factory
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Abstract

The invention relates to a corundum zircon brick (CAZS) which belongs to refractory materials and a manufacturing method thereof, in particular to a corundum zircon brick which is a refractory material with good anti-erosion property and excellent thermal shock property. The corundum zircon brick is generally used for the forming part of a passage of a daily glass kiln. The brick is made from aggregates and matrix materials, wherein the aggregates of the refractory material adopts the coarse and medium particles of sintered plate type corundum, and fine particles of zirconite and electric melting mullite, and the powder used as the matrix materials adopt the superfine particles of the electric melting mullite and the zirconite with the particle size smaller than 400 meshes (38 micrometers). A finished corundum zircon brick product is obtained by a forming process with wet type grouting at moderate firing temperature.

Description

A kind of manufacture method of corundum zircon brick
The field of the invention
The present invention relates to belong to corundum zircon brick (CAZS) and the manufacture method thereof of refractory materials.More particularly, relate to the refractory materials corundum zircon brick that a kind of resistance to fouling is good, thermal shock resistance is good, generally it is used for daily glass furnace path moulding position.
Background technology
Openly also used many bricks of being made by corundum as refractory materials in the prior art.
Chinese patent application 94119419.1 (CN1151389A) discloses the novel oxidation style Technology of a kind of fused cast zirconia-alumina brick, it is characterized in that: (1) electric furnace feeding point is at uniform 3 and feeds intake; (2) the throwing furnace charge of electric furnace is first behind hollow graphite electrode plasma long arc oxidation fusion, again through the oxygen blowing device oxygen blast; Used oxygen blowing device adopts hydrostatic transmission, and automatic lifting swings the oxygen rifle to the interior oxygen blast of stove; (3) molding system adopts sand mold baking far infrared rays resistance stove and self-hardening sand mixing machine, and the assembly unit mould making process of baking sodium silicate sand template is combined with the molded mold technique of unit sand; (4) the pre-assembled bundle of lines diamond of cold working clip machine, rattler, drilling machine and 150 square metres of pre-assembled platforms of high precision are combined, part and whole kiln fused cast zirconia-alumina brick that the pre-assembled all kinds of glass melters of energy are used.Be characterized as three place's electric furnace feeding points, twice oxidation style technique, mould making process is assembly unit and self-contained combining, the cold working system has newly designed 150 square metres of pre-assembled platforms of high precision, part and whole kiln fused cast zirconia-alumina brick that the pre-assembled all kinds of glass melters of energy are used.
Chinese patent application 01145517.9 (CN1418833A) discloses a kind of founding casting non-oxidate containing plate shape material compound zirconium boule refractory brick, comprise rectangle hexahedron, square hexahedron, trapezoidal hexahedron, arc hexahedron, hollow cylinder body, abnormity hexahedron zirconia-corundum refractory brick is characterized in that: with the zirconia-corundum refractory brick of any label of the approximate parallel direction of planation surface in the casting embedding be inclusive with non-oxidized substance sheet material composite bed.Roller lifting hanging arm guiding mechanism for intaglio press can have flange, and its shape is approximate corresponding with refractory brick planation surface shaped wheel profile, and composite material can be metal molybdenum sheet material, or be aluminium nitride sheet material, or be silicon nitride sheet material, or be zirconium boride 99.5004323A8ure sheet material, or be norbide sheet material, or be boron nitride sheet material, or be the grand sheet material of match.The available pure raw material of the beautiful refractory brick brick body material of compound zirconium, or skillful material, or raw material and grog are mixed in proportion, its production method fundamental sum zirconia-corundum refractory brick production method is identical, before cast non-oxidized substance sheet material composite bed is fixed on and waters in the mold cavity, compound zirconia-corundum refractory brick obviously increases the service life, and prolongs glass furnace furnace life, improve glass quality, have obvious economic benefit.
Chinese patent patent application 200410102985.5 (CN1636940A) discloses the manufacture method of zirconia-corundum refractory brick, the method adopts high temperature oxidation aluminium powder, zircon sand, desilicated zirconia, soda ash, borax and waste material (secondary cast material) to prepare zirconia-corundum refractory brick for raw material, content by controlling above-mentioned each component and adopt the method such as in batches melting has been produced low-cost, the measured zirconia-corundum refractory brick of matter.
The open high-strength compact zirconia-chromia corundum brick of Chinese patent application 200610047205.0 (CN1887788A) is by corundum, zirconium material, chromia material, adds wedding agent and makes.Described corundum is two kinds in electric smelting compact alumina and brown corundum, its ratio of components is by weight percentage: compact alumina 10-80%, brown corundum 0-60%, zirconium material 1-25%, chromia material 3-40%, add the 1-12% wedding agent of above-mentioned batching gross weight and make, zirconium dioxide in the zirconium material 〉=95%, chromium sesquioxide in the chromia material 〉=46%, aluminium sesquioxide in the compact alumina composition>99%, 80%<aluminium sesquioxide<99% in the palm fibre corundum composition, the granularity of compact alumina, brown corundum, zirconium material, chromia material is 5mm to 1000 order.
Chinese patent application 200810021976.1 (CN101381236A) discloses a kind of highiy refractory brick, and it comprises the component of following parts by weight: 3~5 parts in 10~12 parts of lapis amiridiss, 6~8 parts of kaolin, 50~56 parts of zircon sands, 13~16 parts of chromium dioxide, 8~10 parts of zirconium dioxides and water.The invention also discloses the technique of the above-mentioned highiy refractory brick of preparation.Highiy refractory brick of the present invention can tolerate 2100 ℃ high temperature, can satisfy the working conditions of High Temperature Furnaces Heating Apparatus fully, and has stronger resistance to erosion, abrasion resistance properties, the advantage of anticorrosive, good thermal shock stability, long service life.Preparation method of the present invention, unique employing double roasting technique make highiy refractory brick of the present invention can satisfy ultra-high temperature condition, and the preparation method is simple, is easy to realize.
Yet the erosion resistance of these zircon bricks of the prior art and heat-shock resistance need further to improve.
Purpose of the present invention
The purpose of this invention is to provide a kind of special corundum products that contains the zircon phase.It is the refractory materials that combines the highly heatproof and shockproof of zircon erosion resistance and corundum phase-mullite phase composite rock phase structure.Specifically, the invention provides a kind of corundum zircon brick (CAZS) and manufacture method thereof.
Technical solution of the present invention
Usually, the corundum zircon product is divided into three kinds according to the difference of composition (weight), and it is composed as follows:
Figure GSA00000119435000031
Generally speaking, its technical indicator composition (weight) of corundum zircon product is as follows:
Al 2O 3ZrO 2Fe 2O 3Total impurities
CAZS:75~68% 9~19% ≤0.50% ≤1.0%
Corundum zircon brick (CAZS) product of the present invention's preparation has good, the good heat-shock resistance of good resistance to fouling.
This product is selected thick, the middle particle of sintering plate corundum, zircon and electrofused mullite be fine particle as the refractory materials skeleton, powder selects the granularity of electrofused mullite and zircon all less than 400 orders (38 microns).Moulding process by wet type grouting is made finished product, and suitable firing temperature obtains with zircon, and the corundum phase is the high-grade refractory materials of master's composite rock phase composite with mullite mutually.
In one embodiment of the invention, provide the manufacture method of corundum zircon brick, it may further comprise the steps:
1) preparation of matrix slurry: with the electrofused mullite powder of crossing 350-450 order (preferred 400 orders (≤38 microns)) sieve of 54~72 weight parts (preferred 60~67), the zircon powder of crossing 350-450 order (preferred 400 orders (≤38 microns)) sieve of 28~46 weight parts (preferred 33~40) is based on the tripoly phosphate sodium STPP (NP as additive of 0.13~0.40 weight part (preferred 0.16~0.30) of the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder 3) or Sodium hexametaphosphate 99 (NP 6), and based on the water glass solution (as activator) of 0.001~0.01 weight part (preferred 0.004~0.008) of the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder (preferred, density 1.36~1.50g/cm 3(being equivalent to degree Beaume 38-48); Technical indicator: SiO 2〉=26%, Na 2O 〉=8.2%), and the water of 18~30 weight parts (preferred 20~25) joins in the shredder and mixedly to turn 3~6 hours, obtains matrix slurry;
2) mix the preparation of pug: with the size-grade distribution of 37~63 weight parts (preferred 45~55) in 3~0.1mm scope, the sintering plate corundum particle of number average particle size 2.0~0.6mm, the size-grade distribution of 0~10 weight part (preferred 3~7 weight parts) is in 0.001~1mm scope, the electrofused mullite particle of number average particle size 0.05~0.6mm, the zircon fine particle of crossing 20-30 order (preferred 24 orders (≤740 microns)) sieve of 5~10 weight parts (preferred 6~8), with 32~43 weight parts (preferred 35~40, more preferably 36~38) above-mentioned matrix slurry joins and stirs 20~30 minutes in the stirrer, makes the mixing pug; Randomly, if necessary, according to the flowability of material, the water that can add 1~6 weight part (preferred 1~2 weight part) stirs in order to be conducive in whipping process.
3) moulding: above-mentioned mixing pug is carried out ageing mixture after about 1~3 hour, uses mould, by the slip casting of two-sided midge method, make the base substrate of different size, dry to moisture content less than 3wt%;
4) roasting: the base substrate that will dry put under the firing temperature under 1480 ℃~1530 ℃, be incubated 5~13 hours in the kiln (preferred 8~12 hours, more preferably 8~10 hours) to carry out roasting.
In general, roasting can be used calcining system commonly used (intensification, insulation and cooling process).
In the preferred case, described roasting is adopted and is undertaken by calcining system shown below:
Heat-up rate
Normal temperature~400 ℃ 5~10 ℃/h
400~1000℃ 10~15℃/h
1000~firing temperature (℃) 15~20 ℃/h
Firing temperature namely 1480~1530 (℃) insulation 5~13h
Firing temperature (℃)~1000 ℃≤40 ℃/h
1000 ℃~normal temperature≤30 ℃/h
For example when under 1520 ℃ firing temperature, being incubated, adopting and undertaken by calcining system shown below:
Heat-up rate
Normal temperature~400 ℃ 5~10 ℃/h
400~1000℃ 10~15℃/h
1000~1520℃ 15~20℃/h
1520 ℃ of insulation 8~12h
1520~1000℃ ≤40℃/h
1000 ℃~normal temperature≤30 ℃/h
Preferably, mould uses gypsum mold when moulding.After insulation, behind the kiln naturally cooling, taking-up can make finished product.
In step 1) under the effect of additive, can guarantee the Uniform Dispersion of powder, the also better intensity that guarantees the cast base substrate.
In addition, can also be adjusted to the granularity of frame material (sintering plate corundum particle) to corresponding scope, moulding obtains the very thin Idiotype product of base wall, such as orifice ring, barrel etc.Its specific embodiments is as follows:
Step 2 at aforesaid method) in, use the size-grade distribution of 48~57 weight parts at the sintering plate corundum particle of 1~0.1mm scope, wherein:
The weight of selecting the sintering plate corundum of 20~30 order particles is 23~26 weight parts; The weight of 30~60 order particles is 15~18 weight parts; The weight of 60~100 order particles is 10~13 weight parts; (weight of 1~0mm) particle is 5~10 weight parts to electrofused mullite.
Particulate material in 58-62 weight part and mud by weight the ratio of 38-42 stir at stirrer, after churning time is 20~30 minutes, make the mixing pug.The process ageing mixture is the goods of plastic all size after 1~3 hour.Various airing base substrates are at roasting in kilns, and firing temperature is not less than 1480 ℃, are not more than 1530 ℃, be incubated after 8~10 hours, with behind the kiln naturally cooling, can make finished product.
In this application, the particle size distribution of various particles (for example 1mm-0.01mm) can be determined by using two layers of vibratory screening apparatus.The particle that keeps at the second layer is exactly the particle with described size-grade distribution.
The prepared brick product of the present invention carries out under the static state (1450 ℃ of anti-glass (soda-lime glass) erosion tests, constant temperature 36 hours), recording metal line place one direction erosion amount (mm/24h) is≤0.90mm that 1/2nd places one direction erosion amount (mm/24h) are≤0.06mm under the metal line.
In addition, corundum zircon brick of the present invention carries out heat-shock resistance (water quick cooling method) test (test method: YB/T376.1-1995) (1100 ℃, water-cooled), 15 times, N/D.
Embodiment
Embodiment 1
The preparation of matrix slurry: with the electrofused mullite powder of mistake 400 orders (38 microns) of 67.5 weight parts (or 6.75kg) sieve, 32.5 the zircon powder of mistake 400 orders (38 microns) of weight part (or 3.25kg) sieves is based on the tripoly phosphate sodium STPP (NP of 0.2 weight part (or 0.02kg) of the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder 3) or Sodium hexametaphosphate 99 (NP 6), and based on water glass solution (the density 1.36-1.50g/cm of the 0.001-0.01 weight part of the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder 3, be equivalent to degree Beaume 38-48; Technical indicator: SiO 2〉=26%, Na 2O 〉=8.2% etc.), and the water of 25 weight parts (or 2.5kg) joins in the shredder and mixedly to turn 4 hours, obtains matrix slurry;
Mix the preparation of pug: be the sintering plate corundum particle of 1.2mm in 3~0.1mm scope, number average particle size with the size-grade distribution of 52 weight parts (5.2kg), the size-grade distribution of 6 weight parts (0.6kg) is the electrofused mullite particle of 0.45mm in 0.001~1mm scope, number average particle size, the zircon fine particle of mistake 24 orders (≤740 microns) sieve of 5 weight parts (0.5kg), join in the stirrer with the above-mentioned matrix slurry of 37 weight parts (3.7kg) and to stir 25 minutes, make the mixing pug.
Moulding: above-mentioned mixing pug was carried out the about 1-3 of ageing mixture hour, uses gypsum mold, by the slip casting of two-sided midge method, make base substrate, dry to moisture content less than 3wt%;
Roasting: the base substrate that will dry is put in the kiln and be incubated 9 hours to carry out roasting under the firing temperature under 1520 ℃.
This roasting is undertaken by calcining system shown below:
Intensification/cooling rate
Normal temperature~400 ℃ 5~10 ℃/h
400~1000℃ 10~15℃/h
1000~1520℃ 15~20℃/h
1520 ℃ of insulation 9h
1520~1000℃ ≤40℃/h
1000 ℃~normal temperature≤30 ℃/h
Embodiment 2~9
Repeat the program of embodiment 1, make corundum zircon brick according to following condition.
1. the batching of substrate material: prepare substrate material by proportion scale shown in the formula table 1: the size-grade distribution of the fine grinding electrofused mullite material that wherein adopts is 1~20 micron, and the size-grade distribution of zircon powder is 1~20 micron.Identical among activator and its consumption and the embodiment 1.
Table 1 matrix allocation sheet
Figure GSA00000119435000061
Figure GSA00000119435000071
2. wet method fine grinding: put into simultaneously ball mill with the water of 25 weight parts after the batching and carry out fine grinding and mix.
3. mix the pug batching: prepare the mixing pug by proportion scale shown in the formula table 2: wherein adopt the size-grade distribution of plate diamond spar in 3~0.1mm or 1~0.1mm scope, the size-grade distribution of electrofused mullite material is in 1~0.001mm scope, and the size-grade distribution of zircon aggregate is in 1~0.001mm scope.
Table 2 mixes the pug allocation sheet
Figure GSA00000119435000072
4. plaster mould moulding: carry out moulding by the conventional grouting method in this area.
5. airing: the present invention adopts the method for nature airing, airing to moisture content less than 3wt%.
6. burn till: undertaken by calcining system shown below.
Normal temperature~400 ℃ 5~10 ℃/h
400~1000℃ 10~15℃/h
1000~1520℃ 15~20℃/h
1520 ℃ of insulation 10h
1520~1000℃ ≤40℃/h
1000 ℃~normal temperature≤30 ℃/h
7. precision work: the product that burns till is processed by client's requirement.
8. packing is dispatched from the factory.
Under Table A: CAM-S, the CAM-D of corundum zircon of the present invention (CAZS) and prior art, the static state of MZ-20 anti-glass (soda-lime glass) erosion test as a result the time than table
Title Metal line place one direction erosion amount (mm/24h) / 2nd place's one direction erosion amounts (mm/24h) under the metal line Temperature condition (℃) Constant temperature (h)
CAZS-B (embodiment 1) 0.88 0.05 1450 36
CAZS-C (embodiment 2) 1.05 0.09 1450 36
CAM-S (contrast) ≥3.57 Erosion amount can't be measured greatly 1450 36
CAM-D (contrast) 2.28 1.60 1450 36
MZ-20 (contrast) 1.14 0.30 1450 36
Table B: ratio table when CAM-S, the CAM-D of corundum zircon of the present invention (CAZS) and prior art, MZ-20 heat-shock resistance (water quick cooling method) test-results
Title Thermal shock resistance Test conditions Operative norm
CAZS-B (embodiment 1) 15 times, N/D 1100 ℃, water-cooled YB/T 376.1-1995
CAZS-C (embodiment 2) 15 times, N/D 1100 ℃, water-cooled YB/T 376.1-1995
CAM-S (contrast) 15 times, N/D 1100 ℃, water-cooled YB/T 376.1-1995
CAM-D (contrast) 15 times, N/D 1100 ℃, water-cooled YB/T 376.1-1995
MZ-20 (contrast) 10 times, damaged 30% 1100 ℃, water-cooled YB/T 376.1-1995
The above embodiments of the present invention are can not limit the present invention to explanation of the present invention, in the implication suitable with solution of the present invention and any change and the combination in the scope, all should think in the scope of solution of the present invention.

Claims (6)

1. the manufacture method of corundum zircon brick, it may further comprise the steps:
1) preparation of matrix slurry: with the electrofused mullite powder of crossing the 350-450 mesh sieve of 54~72 weight parts, the zircon powder of crossing the 350-450 mesh sieve of 28~45 weight parts, tripoly phosphate sodium STPP or Sodium hexametaphosphate 99 based on 0.13~0.40 weight part of the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder, with 0.001~0.01 water glass solution based on the gross weight of the electrofused mullite powder of 100 weight parts and zircon powder, join with the water of 20~30 weight parts and mixedly in the shredder to turn 3~6 hours, obtain matrix slurry;
2) mix the preparation of pug: with the size-grade distribution of 37~63 weight parts sintering plate corundum particle at 3~0.1mm scope, number average particle size 2.0~0.6mm, the size-grade distribution of 0~10 weight part is at the electrofused mullite particle of 0.001~1mm scope, number average particle size 0.05~0.6mm, the zircon fine particle of crossing the 20-30 mesh sieve of 5~10 weight parts, join with the above-mentioned matrix slurry of 32~43 weight parts and to stir 20~30 minutes in the stirrer, make the mixing pug; Randomly, according to the flowability of material, the water that adds 1~6 weight part stirs in order to be conducive in whipping process;
3) moulding: above-mentioned mixing pug was carried out ageing mixture after 1~3 hour, uses mould, by the slip casting of two-sided midge method, make the base substrate of different size, dry to moisture content less than 3wt%;
4) roasting: the base substrate that will dry is put in the kiln and be incubated 5~13 hours to carry out roasting under the firing temperature under 1480 ℃~1530 ℃.
2. according to claim 1 method, wherein in step 2) in: use the size-grade distribution of 48~57 weight parts at the sintering plate corundum particle of 1~0.1mm scope, number average particle size 0.8~0.6mm, wherein the weight of 20~30 purpose sintering plate corundum particles is 23~26 weight parts; The weight of the particle of 30 orders~60 purpose sintering plate corundum particles is 15~18 weight parts; The weight of the particle of 60 orders~100 purpose sintering plate corundum particles is 10~13 weight parts; With the weight of electrofused mullite particle size-grade distribution 1~0.001mm, number average particle size 0.05~0.6mm be 5~10 weight parts; Wherein particulate material in 58~62 weight parts and mud by weight 38~42 ratio stir at stirrer, stir after 20~30 minutes, make the mixing pug.
3. according to claim 1 and 2 method, wherein said roasting adopts following calcining system to carry out:
Figure FSB00000961662800021
4. the corundum zircon brick that is obtained by the method for any one among the claim 1-3.
5. the corundum zircon brick of claim 4, wherein this brick product carries out heat-shock resistance test, 15 N/Ds, test method: YB/T 376.1-1995,1100 ℃, water quick cooling method.
6. claim 4 or 5 corundum zircon brick, wherein this brick product is by static lower soda-lime glass erosion test, 1450 ℃, constant temperature 36 hours, record metal line place one direction erosion amount, mm/24h, for≤0.90mm, / 2nd place's one direction erosion amounts under the metal line, mm/24h, for≤0.06mm.
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