CN101691305A - Corundum-mullite ceramics cast product and method for preparing same - Google Patents

Corundum-mullite ceramics cast product and method for preparing same Download PDF

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Publication number
CN101691305A
CN101691305A CN200910172488A CN200910172488A CN101691305A CN 101691305 A CN101691305 A CN 101691305A CN 200910172488 A CN200910172488 A CN 200910172488A CN 200910172488 A CN200910172488 A CN 200910172488A CN 101691305 A CN101691305 A CN 101691305A
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sio
corundum
powder
granularity
mullite
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CN200910172488A
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CN101691305B (en
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谭清华
耿可明
吴爱军
朱德先
张涛
胡飘
王晗
张亚栋
吕世坪
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention relates to a corundum-mullite ceramics cast product applied in the industry of white titanium pigment and a method for preparing the same. In the preparation method, SiO2 nanometer powder with a grain size less than 50nm and Al2O3 nanometer powder with a grain size less than 80nm are used as additives, and fine powder of finished ores of andalusite and a highly efficient water reducing agent are introduced to develop the high-thermal shock corundum-mullite ceramics product which can be used for a long time at a high temperature of 1,700 DEG C, is high in anti-bending and pressure withstanding strength and good in washing resistance and corrosion resistance and can also withstand rapid temperature change.

Description

A kind of corundum-mullite cast product and preparation method thereof
Technical field
The present invention relates to a kind of corundum-mullite product that is applied to the titanium dioxide industry and preparation method thereof, specifically, relate to a kind of interpolation SiO 2Nano powder, Al 2O 3Corundum-mullite cast product of nano powder, andaluzite concentrate fine powder and high efficiency water reducing agent and preparation method thereof.
Background technology
Need use a kind of shape and structure complexity in the titanium white production industry, the large-scale refractorily lined material that globality is had relatively high expectations, the handling characteristics of this material is high temperature resistant, corrosion-resistant, high pressure resistant, antiscour, and good volume stability and thermal shock resistance will be arranged, take all factors into consideration think cost performance rationally, the refractory materials that is easy to moulding and can satisfies the titanium white production working conditions is low cement bonded corundum-mullite cast product.
The low-cement refractory pouring goods are refractory materialss of new generation that 20 th century later obtain fast development, it integrates the advantage of multiple refractory castable, have characteristics such as high-density, high strength, low pore, wear-resistant, heat-resisting shake, anti-erosion and impermeabilisation, also have characteristics such as the strong and construction water amount of volume stability is low simultaneously and be widely used, result of use is better and economic results in society are remarkable.And continuing to bring out along with high-quality, high-performance, GOOD TASTE raw material, the introducing of high efficiency water reducing agent, additive and wedding agent etc., the optimization of particle size distribution, the employing of novel mixing equipment, preparation of construction and advanced constructional method, the ambiguity refractory materials is very active in the development of aspects such as material, kind, performance, construction, application, and product innovation emerges in an endless stream.The particularly application of silica alumina micro mist etc., make traditional high cement develop to low cement (ultra-low cement or non-cement), low-moisture mould material direction in conjunction with mould material, ultimate principle is: partly replace cement with super-fine powder, replaced the combination of water and cement granules, make low cement deposit material be easy to flow, water consumption reduces, and void content reduces, and density and intensity are increased.
The continuous promotion and application of the nanotechnology that development in recent years is got up, efficient dispersion technology, and the reinforcement of fundamental research such as the theory of stability (dlvo theory) of surfactivity theory, dispersion system and micro-crack extension theory, in the moulding of instructing the refractory casting goods with to improve on aspect of performance, particularly rheological, coking property, high-temperature stability, heat-shock resistance and anti-erosion, the permeability resistance of refractory casting goods effect very remarkable.
Summary of the invention
In order to solve the problem in the utilisation technology, enlarge the range of application of refractory casting goods, the invention provides a kind of corundum-mullite cast product.
The present invention has used the SiO of granularity<50nm 2The Al of nano powder and granularity<80nm 2O 3Nano powder, and introduce andaluzite concentrate fine powder and high efficiency water reducing agent, developed a kind of can be under 1700 ℃ of high temperature life-time service, anti-folding and compressive strength are higher, anti-washing away, anti-erosion, and stand the high thermal shock corundum-mullite cast product of temperature acute variation.
The present invention provides a kind of preparation method of above-mentioned corundum-mullite cast product simultaneously.
A kind of corundum-mullite cast product that the present invention proposes is characterized in that: these goods with the granularity be 5-0.076mm fused white corundum particle, the fused white corundum fine powder of granularity<0.063mm, the electrofused mullite particle of granularity<3mm, α-Al of granularity<3 μ m 2O 3The SiO of micro mist, granularity<1 μ m 2The andaluzite fine powder of micro mist, granularity<0.063mm and cement are main raw material, with the SiO of granularity<50nm 2The Al of nano powder and granularity<80nm 2O 3Nano powder is an additive, introduces an amount of high efficiency water reducing agent simultaneously;
The composition of corundum-mullite cast product of the present invention (mass percent):
Fused white corundum particle 52~68%
Fused white corundum fine powder 7~15%
Electrofused mullite particle 8~10%
α-Al 2O 3Micro mist 6~10%
SiO 2Micro mist 1~3%
Andaluzite fine powder 3~5%
Cement 3~5%
SiO 2Nano powder 0.5~2%
Al 2O 3Nano powder 0.5~3%
Water reducer (adding) 0.05~0.2%
The requirement of the chemical ingredients of fused white corundum is among the present invention: Al 2O 3〉=99.0%; SiO 2What micro mist adopted is the import micro mist, and its chemical ingredients requirement is: SiO 2〉=97.5%; What cement adopted is pure calcium aluminate cement, and its chemical ingredients requirement is: Al 2O 3〉=70.0%; Electrofused mullite adopts is raw material after the overpickling deironing, its chemical ingredients require be: Al 2O 3+ SiO 2〉=98.0%; It is the andaluzite concentrate that the andaluzite fine powder adopts, and its chemical ingredients requirement is: Al 2O 3+ SiO 2〉=98.8%; SiO 2The chemical ingredients of nano powder requires: SiO 2〉=99.9%; Al 2O 3The nano powder chemical ingredients requires: Al 2O 3〉=99.9%.
Described high efficiency water reducing agent refers to polyocarboxy acid type high efficiency water reducing agent, sulfamate series high-efficiency water-reducing agent or naphthalene series high-efficiency water-reducing agent.
Al in the goods of the present invention 2O 3Total mass percent requires greater than 90%.
The preparation method of above-mentioned corundum-mullite product comprises the steps:
(1) pre-mixing of matrix powder:, comprising: fused white corundum fine powder, α-Al with described fine powder 2O 3Micro mist, SiO 2Micro mist, andaluzite concentrate fine powder, cement, SiO 2Nano powder, Al 2O 3Nano powder, high efficiency water reducing agent were put into the ball mill mixing 30-50 minute, so that SiO according to the ratio of setting 2Nano powder and Al 2O 3The nano powder thorough mixing is even, and it is stand-by that the back is preserved in mixed matrix powder sealing;
The fused white corundum particle that (2) will take by weighing, electrofused mullite particle and the matrix powder that is pre-mixed are put into forced mixer and were mixed 5~10 minutes, after adding the water mixing and stirring that accounts for material gross weight 4~6%, inject the mould that cleaning is clean and fix, be placed on vibrating forming or use vibrating head layering vibrating forming on the shaking table, treat to get final product after the surperficial bleeding;
(3) the maintenance demoulding in 2~4 days behind the casting, under 110~130 ℃ of temperature dry 24~48 hours subsequently, treat that moisture is fully discharged after, goods are burnt till in 1550 ℃ in shuttle kiln, the goods after the burning can use after selection and packing.
The present invention has the performance and the characteristics of following excellence:
(1) owing to adopts SiO 2Nano powder and Al 2O 3The use of nano powder makes nano powder partly replace cement, and the combination that replaces water and cement becomes and is more prone to, and has reduced the void content of cast product, and low temperature density and intensity are increased; Because SiO 2Nano powder and Al 2O 3The granularity of nano powder is thinner, activity is bigger, more uniform characteristics distribute during pre-mixing in earlier stage, during pyroprocessing, making the sintering of cast product become is more prone to, the mullitization of its internal organizational structure is more even, help improving high temperature density, intensity and the thermal shock resistance of cast product, and then improve the antiscour and the erosion-resisting characteristics of cast product, improved its work-ing life.
(2) use of high efficiency water reducing agent has significantly reduced the amount of water of mould material, has improved the flowability of low cement deposit material on the one hand; Increase the density of mould material on the other hand, improved physical strength.
(3) utilize the tiny crack of andaluzite and fused white corundum, the inconsistent generation of electrofused mullite hot expansibility, improve the thermal shock resistance of cast product; The size of utilizing andaluzite high temperature mullitization to produce simultaneously expands and eliminates the dimensional contraction that the corundum-mullite cast product produces because of sintering, so that reduce the dimensional change and the high volume stability of improving cast product of cast product.
Embodiment
Following indefiniteness embodiment is used for explaining in detail production technique of the present invention and technical scheme.In these embodiments, the performance of goods adopts national standard or industry standard to measure more, as volume density, apparent porosity, line velocity of variation, compressive strength and thermal shock resistance etc.
Embodiment 1: the mass percent of each component is: the fused white corundum particle 57% of 0.076-5mm,<the fused white corundum fine powder 13% of 0.063mm, the electrofused mullite particle 10% of 1-3mm, granularity<3 μ m active alpha-Al 2O 3The SiO of micro mist 7%, granularity<1 μ m 2The SiO of micro mist 2.5%, granularity<50nm 2The Al of nano powder 0.5%, granularity<80nm 2O 3Nano powder is 2%,<the andaluzite concentrate fine powder of 0.047mm is 3%, pure calcium aluminate cement 5%, polyocarboxy acid type (ECONEXEPC150 type) high efficiency water reducing agent 0.05% (adding).
The preparation method of above-mentioned corundum-mullite product comprises the steps:
(1) pre-mixing of matrix powder:, comprising: fused white corundum fine powder, α-Al with described fine powder 2O 3Micro mist, SiO 2Micro mist, andaluzite concentrate fine powder, cement, SiO 2Nano powder, Al 2O 3Nano powder, high efficiency water reducing agent are put into ball mill and were mixed 40 minutes, so that SiO according to the ratio of setting 2Nano powder and Al 2O 3The nano powder thorough mixing is even, and it is stand-by that the back is preserved in mixed matrix powder sealing;
The fused white corundum particle that (2) will take by weighing, electrofused mullite particle and the matrix powder that is pre-mixed are put into forced mixer and were mixed 10 minutes, after adding the water mixing and stirring that accounts for material gross weight 5%, inject the mould that cleaning is clean and fix, be placed on vibrating forming or use vibrating head layering vibrating forming on the shaking table, treat to get final product after the surperficial bleeding;
(3) the maintenance demoulding in 2 days behind the casting, under 110 ℃ of temperature dry 48 hours subsequently, treat that moisture is fully discharged after, goods are burnt till in 1550 ℃ in shuttle kiln, the goods after the burning can use after selection and packing.
Embodiment 2: the mass percent of each component is: the fused white corundum particle 59% of 0.076-5mm,<the fused white corundum fine powder 15% of 0.063mm, the electrofused mullite particle 8% of 0-1mm, granularity<3 μ m active alpha-Al 2O 3The SiO of micro mist 6%, granularity<1 μ m 2The SiO of micro mist 2%, granularity<50nm 2The Al of nano powder 1%, granularity<80nm 2O 3Nano powder is 1%,<the andaluzite concentrate fine powder of 0.047mm is 3%, pure calcium aluminate cement 5%, sulfamate system (YFN-201 type) high efficiency water reducing agent 0.1% (adding).
Embodiment 3: the mass percent of each component is: the fused white corundum particle 57% of 0.076-5mm,<the fused white corundum fine powder 10% of 0.063mm, the electrofused mullite particle 10% of 0-1mm,, granularity<3 μ m active alpha-Al 2O 3The SiO of micro mist 10%, granularity<1 μ m 2The SiO of micro mist 2%, granularity<50nm 2The Al of nano powder 1.5%, granularity<80nm 2O 3Nano powder is 1.5%,<the andaluzite concentrate fine powder of 0.047mm is 3%, pure calcium aluminate cement 5%, naphthalene series high-efficiency water-reducing agent (FDN) 0.2% (adding).
Embodiment 4: the mass percent of each component is: the fused white corundum particle 63% of 0.076-5mm,<the fused white corundum fine powder 8% of 0.063mm, the electrofused mullite particle 8% of 1-3mm, granularity<3 μ m active alpha-Al 2O 3The SiO of micro mist 7%, granularity<1 μ m 2The SiO of micro mist 1%, granularity<50nm 2The Al of nano powder 2%, granularity<80nm 2O 3Nano powder is 3%,<the andaluzite concentrate fine powder of 0.047mm is 5%, pure calcium aluminate cement 3%, polyocarboxy acid type high efficiency water reducing agent (HK-1 type) 0.15% (adding).
Embodiment 5: the mass percent of each component is: the fused white corundum particle 61% of 0.076-5mm,<the active active alpha-Al of the fused white corundum fine powder 7% of 0.063mm, the electrofused mullite particle 9% of 0-1mm, granularity<3 μ m 2O 3The SiO of micro mist 10%, granularity<1 μ m 2The SiO of micro mist 3%, granularity<50nm 2The Al of nano powder 1.5%, granularity<80nm 2O 3Nano powder is 0.5%,<the andaluzite concentrate fine powder of 0.047mm is 5%, pure calcium aluminate cement 3%, sulfamate series high-efficiency water-reducing agent (ZX-B type) 0.1% (adding).
The preparation method of embodiment 2~5 is with embodiment 1.
Performance index see the following form:
Physical and chemical index Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Compressive strength (110 ℃ * 48h), MPa ??41 ??43 ??45 ??38 ??35
Folding strength (110 ℃ * 48h), MPa ??8 ??11 ??9 ??9 ??7
Compressive strength (1550 ℃ * 3h), MPa ??127 ??146 ??120 ??133 ??124
Folding strength (1550 ℃ * 3h), MPa ??33 ??38 ??32 ??35 ??30
Volume density (1550 ℃ * 3h), g/cm 3 ??3.10 ??3.17 ??3.08 ??3.13 ??3.10
Apparent porosity (1550 ℃ * 3h), % ??15.64 ??15.17 ??15.88 ??15.12 ??15.72
The line velocity of variation (1550 ℃ * 3h), % ??-0.28 ??-0.47 ??-0.32 ??-0.25 ??-0.20
Physical and chemical index Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Goods (1550 ℃ * 3h) thermal shock resistance (1100 ℃, water-cooled), inferior ??≥15 ??≥15 ??≥15 ??≥15 ??≥15

Claims (5)

1. corundum-mullite cast product is characterized in that: these goods with the granularity be 5-0.076mm fused white corundum particle, the fused white corundum fine powder of granularity<0.063mm, the electrofused mullite particle of granularity<3mm, α-Al of granularity<3 μ m 2O 3The SiO of micro mist, granularity<1 μ m 2The andaluzite fine powder of micro mist, granularity<0.063mm and cement are main raw material, with the SiO of granularity<50nm 2The Al of nano powder and granularity<80nm 2O 3Nano powder is an additive, introduces an amount of high efficiency water reducing agent simultaneously;
The composition of corundum-mullite cast product of the present invention and mass percent are:
Fused white corundum particle 52~68%
Fused white corundum fine powder 7~15%
Electrofused mullite particle 8~10%
α-Al 2O 3Micro mist 6~10%
SiO 2Micro mist 1~3%
Andaluzite fine powder 3~5%
Cement 3~5%
SiO 2Nano powder 0.5~2%
Al 2O 3Nano powder 0.5~3%
Water reducer (adding) 0.05~0.2%.
2. according to the described a kind of corundum-mullite cast product of claim 1, it is characterized in that: the requirement of the chemical ingredients of fused white corundum is among the present invention: Al 2O 3〉=99.0%; SiO 2What micro mist adopted is the import micro mist, and its chemical ingredients requirement is: SiO 2〉=97.5%; What cement adopted is pure calcium aluminate cement, and its chemical ingredients requirement is: Al 2O 3〉=70.0%; Electrofused mullite adopts is raw material after the overpickling deironing, its chemical ingredients require be: Al 2O 3+ SiO 2〉=98.0%; It is the andaluzite concentrate that the andaluzite fine powder adopts, and its chemical ingredients requirement is: Al 2O 3+ SiO 2〉=98.8%; SiO 2The chemical ingredients of nano powder requires: SiO 2〉=99.9%; Al 2O 3The nano powder chemical ingredients requires: Al 2O 3〉=99.9%.
3. according to the described a kind of corundum-mullite cast product of claim 1, it is characterized in that: described high efficiency water reducing agent refers to polyocarboxy acid type high efficiency water reducing agent or sulfamate series high-efficiency water-reducing agent or naphthalene series high-efficiency water-reducing agent.
4. according to the described a kind of corundum-mullite cast product of claim 1, it is characterized in that: Al in the goods of the present invention 2O 3Total mass percent is greater than 90%.
5. the preparation method of the described corundum-mullite cast product of claim 1, it is characterized in that: described preparation method comprises the steps:
(1) pre-mixing of matrix powder:, comprising: fused white corundum fine powder, α-Al with described fine powder 2O 3Micro mist, SiO 2Micro mist, andaluzite concentrate fine powder, cement, SiO 2Nano powder, Al 2O 3Nano powder, high efficiency water reducing agent were put into the ball mill mixing 30-50 minute, so that SiO according to the ratio of setting 2Nano powder and Al 2O 3The nano powder thorough mixing is even, and it is stand-by that the back is preserved in mixed matrix powder sealing;
The fused white corundum particle that (2) will take by weighing, electrofused mullite particle and the matrix powder that is pre-mixed are put into forced mixer and were mixed 5~10 minutes, after adding the water mixing and stirring that accounts for material gross weight 4~6%, inject the mould that cleaning is clean and fix, be placed on vibrating forming or use vibrating head layering vibrating forming on the shaking table, treat to get final product after the surperficial bleeding;
(3) the maintenance demoulding in 2~4 days behind the casting, under 110~130 ℃ of temperature dry 24~48 hours subsequently, treat that moisture is fully discharged after, goods are burnt till in 1550 ℃ in shuttle kiln, the goods after the burning can use after selection and packing.
CN2009101724885A 2009-10-01 2009-10-01 Corundum-mullite ceramics cast product and method for preparing same Active CN101691305B (en)

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CN101935222A (en) * 2010-08-24 2011-01-05 中钢集团洛阳耐火材料研究院有限公司 High-temperature corundum-porzite pushing plate and manufacture method thereof
CN104193371A (en) * 2014-08-29 2014-12-10 长兴兴鹰新型耐火建材有限公司 Kilneye castable and preparation method thereof
CN105218120A (en) * 2015-11-02 2016-01-06 河南好运祥耐材有限公司 A kind of high-strength and high-ductility wear-resistant castable
CN105218115A (en) * 2015-10-12 2016-01-06 宜兴市炉顶密封工程有限公司 The alkaline-resisting resistance to compression mould material of hard first
CN105272300A (en) * 2015-11-02 2016-01-27 河南好运祥耐材有限公司 Ceramic wear-resistant material for hot fitting
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CN104193371A (en) * 2014-08-29 2014-12-10 长兴兴鹰新型耐火建材有限公司 Kilneye castable and preparation method thereof
CN104193371B (en) * 2014-08-29 2016-09-07 长兴兴鹰新型耐火建材有限公司 A kind of kilneye castable and preparation method thereof
CN105218115A (en) * 2015-10-12 2016-01-06 宜兴市炉顶密封工程有限公司 The alkaline-resisting resistance to compression mould material of hard first
CN105218120A (en) * 2015-11-02 2016-01-06 河南好运祥耐材有限公司 A kind of high-strength and high-ductility wear-resistant castable
CN105272300A (en) * 2015-11-02 2016-01-27 河南好运祥耐材有限公司 Ceramic wear-resistant material for hot fitting
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