CN107032770A - Diffusion-type skeleton enhancing corundum spinelle air brick and preparation method thereof - Google Patents

Diffusion-type skeleton enhancing corundum spinelle air brick and preparation method thereof Download PDF

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CN107032770A
CN107032770A CN201710413603.8A CN201710413603A CN107032770A CN 107032770 A CN107032770 A CN 107032770A CN 201710413603 A CN201710413603 A CN 201710413603A CN 107032770 A CN107032770 A CN 107032770A
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corundum
air brick
diffusion
fine powder
type skeleton
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CN107032770B (en
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李亚伟
梁雄
桑绍柏
徐腾腾
徐义彪
潘丽萍
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Abstract

The present invention relates to a kind of diffusion-type skeleton enhancing corundum spinelle air brick and preparation method thereof.Its technical scheme is：Monoclinic zirconia fine powder, yittrium oxide fine powder, activated alumina fine powder, aluminous cement, ammonium lignosulphonate, polycarboxylate, carboxymethyl cellulose and water are mixed, zirconia slurry is made；Dense sintering corundum in granules, aluminum oxide fine powder, magnesium oxide powder, aluminous cement, polycarboxylate and water are mixed, corundum castable is made.Polyurethane sponge is impregnated in zirconia slurry, extruding or centrifugal drying slurry are dried, and obtain zirconium oxide reticulated porous ceramic biscuit, then are fixed on air brick mold bottom, adds corundum castable, shaping obtains skeleton enhancing corundum spinelle air brick base substrate；Then burnt till at 1500 ~ 1700 DEG C, produce diffusion-type skeleton enhancing corundum spinelle air brick.Present invention process is simple and cost is low, and prepared product through hole is evenly distributed, throughput big, good integrity and thermal shock resistance are excellent.

Description

Diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof
Technical field
The invention belongs to air brick technical field.More particularly to a kind of diffusion-type skeleton enhancing corundum-spinel air brick And preparation method thereof.
Background technology
With the development of clean steel smelting technique, external refining proportion in smelting process is increasing, wherein, bottom It is most also generally one of most ripe furnace outer refining technology that Argon stirring technique, which is,.Air brick is the important function of BOTTOM ARGON BLOWING technology Element, can play a part of homogenizing liquid steel temperature and removal molten steel is mingled with, and be the key for improving high-quality steel quality.It is main at present The air brick air supply device of stream still uses slot-type ventilating brick, but slot-type ventilating brick thermal shock resistance is poor and slit oozes Steel, is easily caused air brick transverse breakage, directly affects the permeability and service life of air brick.Dispersive air brick relative to Slot-type ventilating brick has the advantages that upper gas is fast, through-blowing rate is high and reduces burning oxygen and operated, and can significantly improve usage safety performance.It is right For diffusion-type corundum-spinel air brick, generally accumulate to realize disperse using the not close of particle in preparation process Type through hole, causes the intergranular binding ability of material internal poor, seriously reduces the bulk strength and thermal shock resistance of air brick.
For the intensity and thermal shock resistance that solve diffusion-type corundum-spinel air brick it is poor the problems such as, a kind of " composite ventilating Brick "（CN201620177U）Patented technology, it is that machine pressure dispersive air brick, bottom are non-diffusion-type to disclose a kind of top Composite air bricks, the method make it that the globality of air brick is poor due to the air brick of two kinds of structures is carried out into physics splicing, holds Molten steel is easily caused to air brick internal penetration, the throughput and service life of the air brick is influenceed." tundish disperse formula is breathed freely Brick and preparation method thereof "（CN103787681A）Patented technology, disclose a kind of integrated poured method of utilization forsterite Dispersive air brick is prepared, though dispersive air brick overall performance prepared by the method is good, UNICOM inside the air brick, It is few through stomata so that the throughput of the dispersive air brick of preparation not enough, influences performance.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide that a kind of technique is simple and the low diffusion-type skeleton of cost Strengthen the preparation method of corundum-spinel air brick, the diffusion-type skeleton enhancing corundum-spinel air brick prepared with this method Good integrity, intensity are high, good in thermal shock and throughput are big.
To achieve the above object, the step of the technical solution adopted by the present invention is：
Step 1: by 60 ~ 85wt% monoclinic zirconia fine powder, 12 ~ 30wt% yittrium oxide fine powder, 2 ~ 15wt% active oxidation Aluminium fine powder and 0.5 ~ 2wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 15 ~ 30wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 60 ~ 70wt% dense sintering corundum in granules, 25 ~ 35wt% aluminum oxide fine powder, 2 ~ 7wt% oxidation Magnesium powder and 2 ~ 5wt% aluminous cement mixing, produce compound II.
The polycarboxylate of the II 0.05 ~ 0.2wt% of compound and 3.5 ~ 6wt% water are added into the compound II, 15 ~ 30min is stirred, corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1500 ~ 1700 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 5 ~ 20ppi.
The ZrO of the monoclinic zirconia fine powder2Content >=99.60wt%, granularity≤0.088mm of monoclinic zirconia fine powder.
The Al of the activated alumina fine powder2O3Content >=99wt%, granularity≤0.002mm of activated alumina fine powder.
The Al of the dense sintering corundum in granules2O3Content >=98wt%, the granularity of dense sintering corundum in granules for 0.5 ~ 2mm。
Content of MgO >=98wt% of the magnesium oxide powder, granularity≤0.045mm of magnesium oxide powder.
The Al of the aluminum oxide fine powder2O3Content >=99wt%；Granularity≤0.088mm of the fine powder of the aluminum oxide.
Due to using above-mentioned technical proposal, the present invention compared with prior art, with following good effect：
The present invention is first immersed the polyurethane sponge with three-dimensional net structure in zirconia slurry using Polymeric sponge method, Extruding or centrifugal drying slurry, zirconium oxide reticulated porous ceramic biscuit is made after drying；Then by zirconium oxide reticulated porous ceramic biscuit The center position of ventilative bricks die is fixed on, the corundum castable stirred is reinjected, through vibration moulding, conserved and de- Mould, then 3 ~ 5h is burnt till under the conditions of 1500 ~ 1700 DEG C, and diffusion-type skeleton enhancing corundum-spinel air brick, technique letter is made Single and cost is low.
The present invention is complete by zirconia slurry by Polymeric sponge method first using polyurethane sponge as pore-creating template Sponge hole muscle surface is coated in, zirconium oxide reticulated porous ceramic biscuit is obtained after drying；Then by the mesh structural porous pottery of zirconium oxide Porcelain biscuit is cast for an entirety with corundum castable, burns till obtained diffusion-type skeleton enhancing corundum-spinel through high temperature and breathes freely Brick.Because the present invention is based on burnout substances mould plate technique, ceramic skeleton enhancing and integrated poured technology, prepared diffusion-type bone Frame enhancing corundum-spinel air brick throughput is big, good integrity and thermal shock resistance are excellent.
The present invention is in preparation process, and diffusion-type through hole can be realized inside the hole muscle of zirconium oxide reticulated porous ceramic.Have When machine foam impregnation method prepares zirconium oxide reticulated porous ceramic biscuit, zircon oxide slurry physical efficiency is wrapped completely to polyurethane sponge hole muscle Wrap up in；After the polyurethane sponge as template is being decomposed for 500 ~ 700 DEG C completely, the burning disability of its own is mesh structural porous in zirconium oxide The three-dimensional net structure of lower polyurethane sponge in itself is left in the hole muscle of ceramics, and then assigns diffusion-type skeleton enhancing corundum-point The good aeration of spar air brick.In addition, zirconium oxide reticulated porous ceramic biscuit is cast in corundum castable, can not only Introduce it is three-dimensional run through the through hole of structure, and to corundum after being burnt till as the zirconium oxide reticulated porous ceramic biscuit of skeleton through high temperature Castable plays enhancing and toughening effect.Furthermore, zirconium oxide reticulated porous ceramic skeleton is from corundum castable because different lines is swollen Swollen coefficient, the two kinds of material interfaces strengthened in diffusion-type skeleton inside corundum-spinel air brick form residual compressive stress, can be eventually Only with absorbing the crackle produced when diffusion-type skeleton strengthens corundum-spinel air brick because of cold cycling, diffusion-type is significantly improved Skeleton strengthens the thermal shock resistance of corundum-spinel air brick.
The enhancing and entirety of diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present invention because of zirconium oxide skeleton Moulding by casting, can not only improve diffusion-type skeleton strengthen corundum-spinel air brick throughput and thermal shock resistance, and compared with The dispersive air brick of mechanical pressing can significantly reduce cost and simplify technique.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present invention is after testing：Cold crushing strength be 160 ~ 210MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 9 times；The diffusion-type skeleton strengthens the throughput of corundum-spinel air brick For 13 ~ 20m3/h·0.3MPa。
Therefore, the present invention has technique simple and the characteristics of low cost, prepared diffusion-type skeleton enhancing corundum-point crystalline substance Stone air brick through hole is evenly distributed, throughput big, good integrity and thermal shock resistance are excellent.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain.
It is now that raw material Unify legislation involved by present embodiment is as follows to avoid repeating：
The ZrO of the monoclinic zirconia fine powder2Content >=99.60wt%, granularity≤0.088mm of monoclinic zirconia fine powder.
The Al of the activated alumina fine powder2O3Content >=99wt%, granularity≤0.002mm of activated alumina fine powder.
The Al of the dense sintering corundum in granules2O3Content >=98wt%.
Content of MgO >=98wt% of the magnesium oxide powder, granularity≤0.045mm of magnesium oxide powder.
The Al of the aluminum oxide fine powder2O3Content >=99wt%；Granularity≤0.088mm of the fine powder of the aluminum oxide.
Embodiment 1
A kind of diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof.The tool of preparation method described in the present embodiment Body step is：
Step 1: by 60 ~ 73wt% monoclinic zirconia fine powder, 20 ~ 30wt% yittrium oxide fine powder, 6 ~ 15wt% active oxidation Aluminium fine powder and 0.5 ~ 1.6wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 15 ~ 22wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 60 ~ 66wt% dense sintering corundum in granules, 29 ~ 35wt% aluminum oxide fine powder, 2 ~ 6.2wt% oxygen Change magnesium powder and 2.8 ~ 5wt% aluminous cement mixing, produce compound II.
The polycarboxylate of the II 0.05 ~ 0.2wt% of compound and 4.7 ~ 6wt% water are added into the compound II, 15 ~ 30min is stirred, corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1500 ~ 1620 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 5 ~ 10ppi.
The granularity of the dense sintering corundum in granules is 1 ~ 2mm.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present embodiment 1 is after testing：Cold crushing strength is 165~187MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 8 times；The diffusion-type skeleton strengthens the logical of corundum-spinel air brick Tolerance is 16 ~ 18m3/h·0.3MPa。
Embodiment 2
A kind of diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof.The tool of preparation method described in the present embodiment Body step is：
Step 1: by 63 ~ 76wt% monoclinic zirconia fine powder, 18 ~ 28wt% yittrium oxide fine powder, 5 ~ 14wt% active oxidation Aluminium fine powder and 0.6 ~ 1.7wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 17 ~ 24wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 61 ~ 67wt% dense sintering corundum in granules, 28 ~ 34wt% aluminum oxide fine powder, 2.2 ~ 6.4wt% Magnesium oxide powder and 2.6 ~ 4.8wt% aluminous cement mixing, produce compound II.
The polycarboxylate of the II 0.05 ~ 0.2wt% of compound and 4.45.7wt% water are added into the compound II, 15 ~ 30min is stirred, corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1520 ~ 1640 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 10 ~ 20ppi.
The granularity of the dense sintering corundum in granules is 0.5 ~ 1mm.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present embodiment 2 is after testing：Cold crushing strength is 160~180MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 8 times；The diffusion-type skeleton strengthens the logical of corundum-spinel air brick Tolerance is 17 ~ 20m3/h·0.3MPa。
Embodiment 3
A kind of diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof.The tool of preparation method described in the present embodiment Body step is：
Step 1: by 66 ~ 79wt% monoclinic zirconia fine powder, 16 ~ 26wt% yittrium oxide fine powder, 4 ~ 13wt% active oxidation Aluminium fine powder and 0.7 ~ 1.8wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 19 ~ 26wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 62 ~ 68wt% dense sintering corundum in granules, 27 ~ 33wt% aluminum oxide fine powder, 2.4 ~ 6.6wt% Magnesium oxide powder and 2.4 ~ 4.4wt% aluminous cement mixing, produce compound II.
The polycarboxylate and 4.1 ~ 5.4wt% of the II 0.05 ~ 0.2wt% of compound is added into the compound II Water, stirs 15 ~ 30min, and corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1540 ~ 1660 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 5 ~ 10ppi.
The granularity of the dense sintering corundum in granules is 1 ~ 2mm.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present embodiment 3 is after testing：Cold crushing strength is 170~190MPa；1100 DEG C of Water-cooling circulating number of times are 7 ~ 9 times；The diffusion-type skeleton strengthens the logical of corundum-spinel air brick Tolerance is 13 ~ 17m3/h·0.3MPa。
Embodiment 4
A kind of diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof.The tool of preparation method described in the present embodiment Body step is：
Step 1: by 69 ~ 82wt% monoclinic zirconia fine powder, 14 ~ 24wt% yittrium oxide fine powder, 3 ~ 12wt% active oxidation Aluminium fine powder and 0.8 ~ 1.9wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 21 ~ 28wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 63 ~ 69wt% dense sintering corundum in granules, 26 ~ 32wt% aluminum oxide fine powder, 2.6 ~ 6.8wt% Magnesium oxide powder and 2.2 ~ 4.4wt% aluminous cement mixing, produce compound II.
The polycarboxylate and 3.8 ~ 5.1wt% of the II 0.05 ~ 0.2wt% of compound is added into the compound II Water, stirs 15 ~ 30min, and corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1560 ~ 1680 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 5 ~ 10ppi.
The granularity of the dense sintering corundum in granules is 1 ~ 2mm.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present embodiment 4 is after testing：Cold crushing strength is 185~210MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 8 times；The diffusion-type skeleton strengthens the logical of corundum-spinel air brick Tolerance is 14 ~ 17m3/h·0.3MPa。
Embodiment 5
A kind of diffusion-type skeleton enhancing corundum-spinel air brick and preparation method thereof.The tool of preparation method described in the present embodiment Body step is：
Step 1: by 72 ~ 85wt% monoclinic zirconia fine powder, 12 ~ 22wt% yittrium oxide fine powder, 2 ~ 11wt% active oxidation Aluminium fine powder and 0.9 ~ 2wt% aluminous cement mixing, produce compound I.
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% poly- carboxylic of the I 0.5 ~ 2wt% of compound is added into the compound I The water of hydrochlorate, 0.2 ~ 1wt% carboxymethyl cellulose and 23 ~ 30wt%, stirs 30 ~ 60min, and zirconia slurry is made.
Step 2: by 64 ~ 70wt% dense sintering corundum in granules, 25 ~ 31wt% aluminum oxide fine powder, 2.8 ~ 7wt% oxygen Change magnesium powder and 2 ~ 4.2wt% aluminous cement mixing, produce compound II.
The polycarboxylate and 3.5 ~ 4.8wt% of the II 0.05 ~ 0.2wt% of compound is added into the compound II Water, stirs 15 ~ 30min, and corundum castable is made.
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 12 ~ 24h is dried under the conditions of 90 ~ 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained.
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is netted The center line of porous ceramics biscuit is overlapped with the center line of the dispersive air brick mould；Again to the dispersive air brick mould The corundum castable is added in tool, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate.
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min Speed be warming up to 600 ~ 800 DEG C, then be warming up to 1580 ~ 1700 DEG C with 2 ~ 5 DEG C/min speed, be incubated 3 ~ 5h；Furnace cooling To room temperature, diffusion-type skeleton enhancing corundum-spinel air brick is made.
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, poly- ammonia Any cross-sectional diameter of ester sponge is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；It is described poly- The average pore size of urethane sponge is 10 ~ 20ppi.
The granularity of the dense sintering corundum in granules is 0.5 ~ 1mm.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by the present embodiment 5 is after testing：Cold crushing strength is 160~190MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 7 times；The diffusion-type skeleton strengthens the logical of corundum-spinel air brick Tolerance is 16 ~ 19m3/h·0.3MPa。
Present embodiment compared with prior art, with following good effect：
Polyurethane sponge with three-dimensional net structure is immersed oxygen by present embodiment using Polymeric sponge method first Change in zirconium slurry, zirconium oxide reticulated porous ceramic biscuit is made after drying in extruding or centrifugal drying slurry；Then it is zirconium oxide is netted more Hole biscuit of ceramics is fixed on the center position of ventilative bricks die, reinjects the corundum castable stirred, through vibration moulding, Maintenance and the demoulding, then 3 ~ 5h is burnt till under the conditions of 1500 ~ 1700 DEG C, and diffusion-type skeleton enhancing corundum-spinel is made and breathes freely Brick, technique is simple and cost is low.
Present embodiment is using polyurethane sponge as pore-creating template, first by Polymeric sponge method by zirconium oxide Slurry is entirely coated on sponge hole muscle surface, and zirconium oxide reticulated porous ceramic biscuit is obtained after drying；Then by zirconium oxide net Shape porous ceramics biscuit is cast for an entirety with corundum castable, and burning till obtained diffusion-type skeleton through high temperature strengthens corundum-point Spar air brick.Because present embodiment is based on burnout substances mould plate technique, ceramic skeleton enhancing and integrated poured technology, Prepared diffusion-type skeleton enhancing corundum-spinel air brick throughput is big, good integrity and thermal shock resistance are excellent.
Present embodiment is in preparation process, and diffusion-type through hole can be inside the hole muscle of zirconium oxide reticulated porous ceramic Realize.When Polymeric sponge method prepares zirconium oxide reticulated porous ceramic biscuit, zircon oxide slurry physical efficiency is to polyurethane sponge hole muscle It is fully wrapped around；After the polyurethane sponge as template is being decomposed for 500 ~ 700 DEG C completely, the burning of its own disables in zirconium oxide net The three-dimensional net structure of lower polyurethane sponge in itself is left in the hole muscle of shape porous ceramics, and then it is firm to assign the enhancing of diffusion-type skeleton Jade-good the aeration of spinelle air brick.In addition, zirconium oxide reticulated porous ceramic biscuit is cast in corundum castable, Can not only introduce it is three-dimensional run through the through hole of structure, and after being burnt till as the zirconium oxide reticulated porous ceramic biscuit of skeleton through high temperature Enhancing and toughening effect are played to corundum castable.Furthermore, zirconium oxide reticulated porous ceramic skeleton is with corundum castable because of difference Linear expansion coefficient, diffusion-type skeleton strengthen corundum-spinel air brick inside two kinds of material interfaces formed residual pressure should Power, can terminate and absorb the crackle produced when diffusion-type skeleton strengthens corundum-spinel air brick because of cold cycling, significantly improve Diffusion-type skeleton strengthens the thermal shock resistance of corundum-spinel air brick.
Diffusion-type skeleton prepared by present embodiment strengthens corundum-spinel air brick because of the enhancing of zirconium oxide skeleton And integrated poured shaping, can not only improve diffusion-type skeleton strengthens the throughput and thermal shock resistance of corundum-spinel air brick Can, and can significantly reduce cost compared with the dispersive air brick of mechanical pressing and simplify technique.
Diffusion-type skeleton enhancing corundum-spinel air brick prepared by present embodiment is after testing：The resistance to pressure of normal temperature Spend for 160 ~ 210MPa；1100 DEG C of Water-cooling circulating number of times are 6 ~ 9 times；The diffusion-type skeleton strengthens corundum-spinel air brick Throughput be 13 ~ 20m3/h·0.3MPa。
Therefore, present embodiment has technique simple and the characteristics of cost is low, and prepared diffusion-type skeleton strengthens Corundum-spinel air brick through hole is evenly distributed, throughput big, good integrity and thermal shock resistance are excellent.

Claims (7)

1. a kind of diffusion-type skeleton strengthens the preparation method of corundum-spinel air brick, the step of the preparation method is characterised by Suddenly it is：
Step 1: by 60 ~ 85wt% monoclinic zirconia fine powder, 12 ~ 30wt% yittrium oxide fine powder, 2 ~ 15wt% active oxidation Aluminium fine powder and 0.5 ~ 2wt% aluminous cement mixing, produce compound I；
Ammonium lignosulphonate, the 0.1 ~ 0.5wt% polycarboxylic acids of the I 0.5 ~ 2wt% of compound is added into the compound I The water of salt, 0.2 ~ 1wt% carboxymethyl cellulose and 15 ~ 30wt%, stirs 30 ~ 60min, and zirconia slurry is made；
Step 2: 60 ~ 70wt% dense sintering corundum in granules, 25 ~ 35wt% aluminum oxide fine powder, 2 ~ 7wt% magnesia is thin Powder and 2 ~ 5wt% aluminous cement mixing, produce compound II；
The polycarboxylate of the II 0.05 ~ 0.2wt% of compound and 3.5 ~ 6wt% water are added into the compound II, is stirred 15 ~ 30min, is made corundum castable；
Step 3: polyurethane sponge is immersed in the zirconia slurry, 10 ~ 30min, extruding or centrifugal drying slurry are impregnated, 90 ~ 12 ~ 24h is dried under the conditions of 110 DEG C, zirconium oxide reticulated porous ceramic biscuit is obtained；
The zirconium oxide reticulated porous ceramic biscuit is fixed on dispersive air brick mold bottom, the zirconium oxide is mesh structural porous The center line of biscuit of ceramics is overlapped with the center line of the dispersive air brick mould；Again into the dispersive air brick mould The corundum castable is added, vibration moulding is conserved, the demoulding, obtain skeleton enhancing corundum-spinel air brick base substrate；
Step 4: skeleton enhancing corundum-spinel air brick base substrate is inserted in high temperature furnace, with 0.5 ~ 3 DEG C/min speed Rate is warming up to 600 ~ 800 DEG C, then is warming up to 1500 ~ 1700 DEG C with 2 ~ 5 DEG C/min speed, is incubated 3 ~ 5h；Cool to room with the furnace Temperature, is made diffusion-type skeleton enhancing corundum-spinel air brick；
The polyurethane sponge is in circular cone shape, and the height of polyurethane sponge is 1.1 ~ 1.2 times of air brick height, polyurethane sea Continuous any cross-sectional diameter is 0.7 ~ 0.9 times of the corresponding cross-sectional diameter of ventilative bricks die equal-height position；The polyurethane The average pore size of sponge is 5 ~ 20ppi.
2. diffusion-type skeleton as claimed in claim 1 strengthens the preparation method of corundum-spinel air brick, it is characterised in that institute State the ZrO of monoclinic zirconia fine powder2Content >=99.60wt%, granularity≤0.088mm of monoclinic zirconia fine powder.
3. diffusion-type skeleton as claimed in claim 1 strengthens the preparation method of corundum-spinel air brick, it is characterised in that institute State the Al of activated alumina fine powder2O3Content >=99wt%, granularity≤0.002mm of activated alumina fine powder.
4. diffusion-type skeleton as claimed in claim 1 strengthens the preparation method of corundum-spinel air brick, it is characterised in that institute State the Al of dense sintering corundum in granules2O3Content >=98wt%, the granularity of dense sintering corundum in granules is 0.5 ~ 2mm.
5. diffusion-type skeleton as claimed in claim 1 strengthens the preparation method of corundum-spinel air brick, it is characterised in that institute State content of MgO >=98wt% of magnesium oxide powder, granularity≤0.045mm of magnesium oxide powder.
6. diffusion-type skeleton as claimed in claim 1 strengthens the preparation method of corundum-spinel air brick, it is characterised in that institute State the Al of aluminum oxide fine powder2O3Content >=99wt%；Granularity≤0.088mm of the fine powder of the aluminum oxide.
7. a kind of diffusion-type skeleton strengthens corundum-spinel air brick, it is characterised in that the diffusion-type skeleton strengthens corundum-point Spar air brick is that diffusion-type skeleton strengthens the system of corundum-spinel air brick according to any one of claim 1 ~ 6 Diffusion-type skeleton enhancing corundum-spinel air brick prepared by Preparation Method.
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CN111039695A (en) * 2020-01-10 2020-04-21 中钢集团洛阳耐火材料研究院有限公司 Preparation method of silicon carbide rubbing skeleton structure reinforced alumina porous ceramic
CN115321999A (en) * 2022-09-06 2022-11-11 宜兴市隆昌耐火材料有限公司 Preparation method of light refractory zirconia-corundum composite castable

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