CN103979988A - Sialon bonded andalusite/sillimanite/SiC refractory material and preparation method - Google Patents
Sialon bonded andalusite/sillimanite/SiC refractory material and preparation method Download PDFInfo
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- CN103979988A CN103979988A CN201410228451.0A CN201410228451A CN103979988A CN 103979988 A CN103979988 A CN 103979988A CN 201410228451 A CN201410228451 A CN 201410228451A CN 103979988 A CN103979988 A CN 103979988A
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Abstract
The invention discloses a sialon bonded andalusite/sillimanite/SiC refractory material and a preparation method, and belongs to the field of a refractory material. The refractory material comprises the following raw materials: andalusite, sillimanite, alpha-Al2O3 powder, polycrystalline silicon waste and aluminum powder, and dextrin and phenolic resin are taken as binding agents. The refractory material is produced by the following steps: weighing raw materials and mixing to obtain mud, compressing and moulding, and sintering in a nitrogen atmosphere at 1200-1600 DEG C. According to the product disclosed by the invention, characteristics of andalusite and sillimanite are developed and a sialon bonded phase is generated through the polycrystalline silicon waste; the refractory material has the following excellent physical performance indexes: apparent porosity is 9-18%, volume density is 2.5-3.0g/cm<3>, cold crushing strength is 100-300MPa and high temperature bending strength is 20-70MPa, thermal shock resistance, creep resistance, CO resistance and alkaline steam erosion resistance are excellent. The product disclosed by the invention is high in cost performance, and is applicable to the middle upper part of furnace body of a blast furnace. The refractory material is not only favorable for prolonging service life of the blast furnace but also realizes recycling of the polycrystalline silicon waste.
Description
Technical field
The present invention relates to a kind of blast furnace stack middle and upper part refractory materials, relate in particular to a kind of large blast furnace shaft middle and upper part match grand combination andaluzite/sillimanite/SiC composite refractory and preparation method used.
Background technology
Realizing blast furnace long service life, maximizing is the important goal of Iron industry.Along with China's iron and steel metallurgical industry is energy-saving and cost-reducing and deepening constantly with powerful of energy-saving and emission-reduction work advances, it is current problem demanding prompt solution that exploitation adapts to blast furnace longevity refractory materials.Blast-furnace body is divided into furnace throat, shaft, furnace bosh, bosh, cupola well 5 parts from top to bottom.Due to the working conditions difference at each position, also different to the cause for erosion of firebrick lining, this requires the performance of refractory materials to adapt with it.Blast furnace stack middle and upper part refractory materials is bearing violent temperature fluctuation, the erosion of CO, K
2the chemical corrosion of the alkali such as O, NaO steam, this requires corresponding refractory materials to possess following performance: good thermal shock; Normal temperature, hot strength are high; Resistance to CO ability is strong; Alkali resistant steam chemical corrosivity is strong.Blast furnace stack generally adopts corundum-mullite fire resistant materials at present, and large blast furnace adopts Si
3n
4in conjunction with SiC brick or Sialon in conjunction with SiC brick.Si
3n
4be combined with Sialon in conjunction with SiC brick that SiC brick possesses the good performances such as hot strength is high, wear-resisting but price is high, limited its applying at blast furnace.
Kyanite, andaluzite, three kinds of mineral of sillimanite are referred to as " three stones " because chemical composition is identical, physical properties is close with purposes." three stone " mineral are at high temperature all irreversibly converted into mullite and SiO
2, and be attended by volume effect.Because these three kinds of mineral crystal structures are different, thereby it is all not identical to be at high temperature converted into temperature, time, speed and the volume effect of mullite, and the process, form, the crystallization direction that are converted into mullite are also different.It is minimum that kyanite starts invert point, and conversion rate is the fastest and with maximum cubical expansivity; Andaluzite starts greatly to change in the time of 1400 DEG C, and conversion rates is medium, and volume kept stable after changing, and the mullite of formation is medium column or needle-like; Sillimanite transition temperature is the highest, and conversion rates is slow, and volumetric expansion is little, will form short cylinder or acicular mullite.Therefore, adopt suitable sintering temperature, in suitable firing atmosphere, can utilize andaluzite and sillimanite mullitization temperature high, mullitization process character slowly, make goods under use temperature, all have unconverted andaluzite and sillimanite, strengthen creep-resistant property and the high volume stability of goods." three stone " possesses excellent performance, can be used as the basic material of refractory industry or adds modified feedstock, for the production of multiple high refractory brick goods, improves the performance of traditional refractory materials, to meet the particular requirement of hot industry to refractory materials.Zhu Liming etc. are by studying sillimanite and andaluzite to Al
2o
3one SiO
2be the impact of product properties, draw: the Al that adds sillimanite, andaluzite
2o
3one SiO
2be goods, except thermal shock resistance is greatly improved, its cold crushing strength, refractoriness under load, slag resistance etc. also had greatly improved.Wang Xinquan etc. have desirable weave construction taking special grade bauxite grog, brown corundum, high alumina corundum, mullite, sillimanite, andaluzite and clay etc. as the Low Creep High Alumina Bricks of raw material development and production, the own all mullitizations of andaluzite particle in sample, part sillimanite changes mullite into, and mullite is staggered network structure mutually.
China's " three stone " Mineral resources are quite abundant, find nearly hundred places, " three stone " mineral deposit (point) at 25 provinces，municipalities and autonomous regions at present.But " three stone " Mineral resources totally utilize level lower at present, have caused to a certain extent the waste of " three stone " Mineral resources.Therefore, base oneself upon china natural resources advantage, strengthen the Application Areas research of " three stone ", " three stone " product innovation of making great efforts Development of Hi-Tech content, high added value, energy-saving and environmental protection has urgent actual demand and great meaning.
In recent years, the energy, information industry are flourish, also constantly expand as the polysilicon market of main raw material thereupon.But polysilicon can use after need to cutting into silicon chip.Enter cutting slurry at cutting process because the crystalline silicon that has 50%-52% is become silicon powder by cutter damage, cause cutting efficiency to reduce, finally cutting slip inefficacy becomes slug, causes the wasting of resources and environmental pollution, has brought huge pressure to enterprise.Generally adopt at present silicon carbide as cutting abrasive material, therefore cut and in slug, mainly contain HIGH-PURITY SILICON, polyoxyethylene glycol (dispersion agent), silicon carbide and a small amount of metal, but silicon and silicon carbide are in physics and chemistry less, the separation difficulty of difference in nature.Therefore Pure Silicon Metal and silicon carbide, how to recycle cost-effectively in cutting waste material are also current problem demanding prompt solutions.
Summary of the invention
The object of this invention is to provide a kind of good thermal shock, anti-CO and alkali steam aggressiveness is strong, creep-resistant property is excellent, the material of high volume good stability and the preparation method of described material, for blast furnace stack middle and upper part, improve the globality of body of heater, extend the work-ing life of blast furnace, and the exploitation of promotion to andaluzite and sillimanite mineral wealth, realize the recycling of polycrystalline silicon wastes, reduce the production cost of blast furnace stack middle and upper part refractory materials, reduce the wasting of resources and environmental pollution.
Technical scheme of the present invention:
The invention provides a kind of blast furnace stack middle and upper part grand combination andaluzite/sillimanite/SiC of match composite refractory used, by weight percentage, raw material consists of: the andaluzite that 5-15% granularity is 5-3mm, 25-55% granularity is the sillimanite of 3-1mm, 15-35% granularity is 1-0mm sillimanite, 5-30% α-Al
2o
3powder, 5-30% polycrystalline silicon wastes, 0-8% aluminium powder, additional above-mentioned raw materials total amount 1-5% dextrin, 1-6% resol is as bonding agent.
Al in described andaluzite
2o
3>=55%, Fe
2o
3≤ 1.2%, K
2o+Na
2o≤0.5%; Al in described sillimanite
2o
3>=55%, Fe
2o
3≤ 1.2%, K
2o+Na
2o≤0.5%; Described α-Al
2o
3the granularity of powder is 200 orders, α-Al
2o
3middle Al
2o
3>=98%, Fe
2o
3≤ 0.5%, K
2o+Na
2o≤0.5%; Described polycrystalline silicon wastes granularity is discrete distribution, between 1um and 240um, mean particle size is 20um ± 10um, in polycrystalline silicon wastes, contents of free si is 25-60%, and carborundum content is 25-60%, and alumina content is 3-7%, metal Fe content is 1-5%, CaO content is less than 0.5%, MgO content, and to be less than 1%, PEG content be 0.5-3%; The granularity of described aluminium powder is 200 orders, Al>=97% in aluminium powder.
A preparation method for the blast furnace stack middle and upper part grand combination andaluzite/sillimanite/SiC of match composite refractory used, described preparation method comprises the following steps:
A. take various raw materials by described proportioning, powder part is carried out to premix, do time in advance as 30-60min, described powder part comprises that granularity is 1-0mm sillimanite, α-Al
2o
3powder, polycrystalline silicon wastes, aluminium powder.
B. first adding granularity is andaluzite, the 3-1mm sillimanite of 5-3mm, add again 2/3 of the total add-on of bonding agent being formed by dextrin, resol preparing in advance, mix 1-5min, then add the powder and remaining 1/3 bonding agent that in step a, obtain through premix, remix 5-10min.
C. mixture step b being obtained is pressed into firebrick billet through friction press or vibration pressure machine.
D. the firebrick billet of forming is put into 110 ± 10 DEG C of dry 24-48h of moisture eliminator, controlled moisture content below 0.5%.
E. dried adobe is imported to muffle combustion gas nitrogenize shuttle kiln, in 1200-1600 DEG C of nitrogen atmosphere, burn till, finally make the grand combination andaluzite/sillimanite/SiC composite refractory brick of match.
Compared with prior art, feature of the present invention and positively effect:
1. the present invention utilizes Si, Al metal transfer phase technique has been prepared the grand combination andaluzite/sillimanite/SiC composite refractory of match, production technique is simple, identical in conjunction with SiC refractory materials production technique with traditional Si alon, the production unit of refractory materials is not proposed to special requirement, simultaneously taking reserves in China andaluzite abundant and that urgently develop and sillimanite as raw material, not only improve the heat-shock resistance of material, creep-resistant property, the ability that anti-CO and alkali steam corrode, also greatly reduce preparation cost, make product of the present invention there is high performance-price ratio, be conducive to Rapid Popularization and application.
2. the present invention utilizes the difference of andaluzite and sillimanite mullitization transition temperature and rate of expansion, by controlling sintering temperature, make goods under use temperature, all there are unconverted andaluzite and sillimanite to decompose the expansion producing, thereby make inner certain stress that produces of goods, play the effect of opposing loading, the creep-resistant property of strongthener, heat-shock resistance; Give full play to the feature of andaluzite and sillimanite, make goods there is comparatively ideal weave construction: andaluzite particle and sillimanite part change mullite into, pin rod-like mullite is woven into network structure, makes material possess the ability that superior heat-shock resistance, creep resistance, high volume stability and stronger anti-CO and alkali steam corrode.
3. in the grand combination andaluzite/sillimanite/SiC of the match composite refractory that prepared by the present invention, Sialon combination is Si-Al-O-N sosoloid mutually, its solid solubility can change within the specific limits, does not affect the acquisition of the grand combination andaluzite/sillimanite/SiC of last match composite refractory in the time that feed composition slightly changes.Therefore this technique is lower to ingredient requirement, is applicable to industrialization promotion.
4. the grand combination andaluzite/sillimanite/SiC of the match composite refractory that prepared by the present invention possesses good physical performance index.Apparent porosity 9-18%, volume density 2.5-3.0g/cm
3, cold crushing strength 100-300MPa, high temperature break resistant intensity 20-70MPa, refractoriness under load be higher than 1700 DEG C, has good heat-shock resistance, creep resistance and stronger anti-CO, the ability of alkali steam corrosion.
Product of the present invention given full play to andaluzite and sillimanite good thermal shock, anti-CO and alkali steam corrosion ability strong, can under differing temps, change the features such as mullite into, and rationally utilize source abundant, cheap polycrystalline silicon wastes produces Sialon in conjunction with phase, hot strength, oxidation-resistance, the high temperature abrasion resistance of material are improved, not only make product possess high performance-price ratio, also under the prerequisite that does not separate SiC and Si, realize the utilization of polycrystalline silicon wastes, reduced the wasting of resources and environmental pollution.。
6. product of the present invention can be applicable to blast furnace stack middle and upper part, is conducive to reduce the refractory materials kind that blast furnace stack middle and upper part is used, and reduces the workload that body of heater is built by laying bricks or stones, improves the globality of body of heater, improves the work-ing life of blast furnace.
Embodiment
Embodiment 1: match grand combination andaluzite/sillimanite/SiC composite refractory and preparation method that a kind of blast furnace middle and upper part is used, by weight percentage, raw material consists of: the andaluzite that 8% granularity is 5-3mm, 37% granularity is the sillimanite of 3-1mm, 25% granularity is 1-0mm sillimanite, 9% α-Al
2o
3powder, 16% polycrystalline silicon wastes, 2.4% aluminium powder, additional above-mentioned raw materials total amount 2.5% dextrin, 1.2% resol is as bonding agent.
Described preparation method comprises the following steps:
A. take various raw materials by described proportioning, powder part is carried out to premix, do time in advance as 30-60min, described powder part comprises that granularity is 1-0mm sillimanite, α-Al
2o
3powder, polycrystalline silicon wastes, aluminium powder.
B. first adding granularity is the andaluzite of 5-3mm, the sillimanite of 3-1mm, add again 2/3 of the total add-on of bonding agent being formed by dextrin, resol preparing in advance, mix 1-5min, then add the powder and remaining 1/3 bonding agent that in step a, obtain through premix, remix 5-10min.
C. mixture step b being obtained is pressed into firebrick billet through friction press or vibration pressure machine.
D. the firebrick billet of forming is put into 110 DEG C of dry 48h of moisture eliminator, controlled moisture content below 0.5%.
E. dried adobe is imported to muffle combustion gas nitrogenize shuttle kiln, in 1450 DEG C of nitrogen atmospheres, burn till, finally make the grand combination andaluzite/sillimanite/SiC composite refractory brick of match.
Products obtained therefrom performance index are: apparent porosity 10%, volume density 2.81g/cm
3, cold crushing strength 198MPa, high temperature break resistant intensity 50MPa, refractoriness under load>=1700 DEG C, have the ability that good heat-shock resistance, creep resistance and stronger anti-CO and alkali steam corrode.
Embodiment 2: production technique is identical with embodiment 1, and difference is:
By weight percentage, raw material consists of: the andaluzite that 8% granularity is 5-3mm, and the sillimanite that 37% granularity is 3-1mm, 25% granularity is 1-0mm sillimanite, 7.5% α-Al
2o
3powder, 18% polycrystalline silicon wastes, 2.4% aluminium powder, additional above-mentioned raw materials total amount 2.5% dextrin, 1.2% resol is as bonding agent.
Products obtained therefrom performance index are: apparent porosity 12%, volume density 2.78g/cm
3, cold crushing strength 182MPa, high temperature break resistant intensity 40MPa, refractoriness under load>=1700 DEG C, have the ability that good heat-shock resistance, creep resistance and stronger anti-CO and alkali steam corrode.
Claims (3)
1. the grand combination andaluzite/sillimanite/SiC composite refractory of match, it is characterized in that: by weight percentage, raw material consists of: the andaluzite that 5-15% granularity is 5-3mm, the sillimanite that 25-55% granularity is 3-1mm, 15-35% granularity is 1-0mm sillimanite, 5-30% α-Al
2o
3powder, 5-30% polycrystalline silicon wastes, 0-8% aluminium powder, additional above-mentioned raw materials total amount 1-5% dextrin, 1-6% resol are as bonding agent.
2. the grand combination andaluzite/sillimanite/SiC of match according to claim 1 composite refractory, is characterized in that: Al in described andaluzite
2o
3>=55%, Fe
2o
3≤ 1.2%, K
2o+Na
2o≤0.5%; Al in described sillimanite
2o
3>=55%, Fe
2o
3≤ 1.2%, K
2o+Na
2o≤0.5%; Described α-Al
2o
3the granularity of powder is 200 orders, α-Al
2o
3middle Al
2o
3>=98%, Fe
2o
3≤ 0.5%, K
2o+Na
2o≤0.5%; The granularity of described polycrystalline silicon wastes is discrete distribution, between 1um and 240um, mean particle size is 20um ± 10um, in polycrystalline silicon wastes, contents of free si is 25-60%, and carborundum content is 25-60%, and alumina content is 3-7%, metal Fe content is 1-5%, CaO content is less than 0.5%, MgO content, and to be less than 1%, PEG content be 0.5-3%; The granularity of described aluminium powder is 200 orders, Al>=97% in aluminium powder.
3. the preparation method of the grand combination andaluzite/sillimanite/SiC of the match described in claim 1 or 2 composite refractory, is characterized in that:
A. take various raw materials by described proportioning, powder part is carried out to premix, do time in advance as 30-60min, described powder part comprises that granularity is 1-0mm sillimanite, α-Al
2o
3powder, polycrystalline silicon wastes, aluminium powder;
B. first adding granularity is andaluzite, the 3-1mm sillimanite of 5-3mm, add again 2/3 of the total add-on of bonding agent being formed by dextrin, resol preparing in advance, mix 1-5min, then add the powder and remaining 1/3 bonding agent that in step a, obtain through premix, remix 5-10min;
C. mixture step b being obtained is pressed into firebrick billet through friction press or vibration pressure machine;
D. the firebrick billet of forming is put into 110 ± 10 DEG C of dry 24-48h of moisture eliminator, controlled moisture content below 0.5%;
E. dried adobe is imported to muffle combustion gas nitrogenize shuttle kiln, in 1200-1600 DEG C of nitrogen atmosphere, burn till, finally make the grand combination andaluzite/sillimanite/SiC composite refractory brick of match.
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|---|---|---|---|
| CN201410228451.0A CN103979988B (en) | 2014-05-27 | 2014-05-27 | Sialon bonded andalusite/sillimanite/SiC refractory material and preparation method |
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| CN103979988B CN103979988B (en) | 2015-04-22 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220194A (en) * | 2016-07-11 | 2016-12-14 | 雷春生 | A kind of preparation method of low creep anti-thermal shock burner block |
| CN109293373A (en) * | 2018-10-23 | 2019-02-01 | 河南省衡锐佳新材料科技有限公司 | A kind of preparation of environment-friendly silicon-based additive and the application method in refractory material |
| CN115286404A (en) * | 2022-08-23 | 2022-11-04 | 宜兴瑞泰耐火材料有限公司 | Low-aluminum mullite castable for molybdenum-containing waste liquid incinerator and preparation method thereof |
| CN116675545A (en) * | 2023-06-02 | 2023-09-01 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of corrosion-penetration-resistant high-purity zirconia refractory product |
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| JP2007277349A (en) * | 2006-04-04 | 2007-10-25 | Kurosaki Harima Corp | Alumina-silica brick for cdq |
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| CN102557713A (en) * | 2011-12-27 | 2012-07-11 | 济南圣泉倍进陶瓷过滤器有限公司 | Ceramic foam filter, composition for preparing ceramic foam filter and preparation method for ceramic foam filter |
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2014
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| US5972102A (en) * | 1996-10-29 | 1999-10-26 | North American Refractories Co. | Hydraulically-bonded monolithic refractories containing a calcium oxide-free binder comprised of a hydratable alumina source and magnesium oxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220194A (en) * | 2016-07-11 | 2016-12-14 | 雷春生 | A kind of preparation method of low creep anti-thermal shock burner block |
| CN109293373A (en) * | 2018-10-23 | 2019-02-01 | 河南省衡锐佳新材料科技有限公司 | A kind of preparation of environment-friendly silicon-based additive and the application method in refractory material |
| CN109293373B (en) * | 2018-10-23 | 2021-05-28 | 河南省衡锐佳新材料科技有限公司 | Preparation of environment-friendly silicon-based additive and application method of environment-friendly silicon-based additive in refractory material |
| CN115286404A (en) * | 2022-08-23 | 2022-11-04 | 宜兴瑞泰耐火材料有限公司 | Low-aluminum mullite castable for molybdenum-containing waste liquid incinerator and preparation method thereof |
| CN116675545A (en) * | 2023-06-02 | 2023-09-01 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of corrosion-penetration-resistant high-purity zirconia refractory product |
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