CN103979988B - 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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- CN103979988B CN103979988B CN201410228451.0A CN201410228451A CN103979988B CN 103979988 B CN103979988 B CN 103979988B CN 201410228451 A CN201410228451 A CN 201410228451A CN 103979988 B CN103979988 B CN 103979988B
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- andaluzite
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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, particularly relate to the match used of a kind of large blast furnace shaft middle and upper part grand in conjunction with andaluzite/sillimanite/SiC composite refractory and preparation method.
Background technology
Realizing prolonging campaign, maximizing is the important goal of Iron industry.Along with China's iron and steel metallurgical industry is saved energy and reduce the cost and the deepening constantly and powerful to advance of energy-saving and emission-reduction work, it is current problem demanding prompt solution that exploitation adapts to prolonging campaign refractory materials.Blast-furnace body is divided into furnace throat, shaft, furnace bosh, bosh, cupola well 5 part from top to bottom.Because the working conditions at each position is different, also different to the cause for erosion of firebrick lining, this requires that the performance of refractory materials adapts with it.Blast furnace stack middle and upper part refractory materials subjects violent temperature fluctuation, the erosion of CO, K
2the chemical corrosion of the alkali steam such as O, NaO, this requires that corresponding refractory materials possesses following performance: good thermal shock; Normal temperature, hot strength are high; Resistance to CO ability is strong; Alkali resistant steam chemical corrosivity is strong.Current blast furnace stack generally adopts corundum-mullite fire resistant materials, and large blast furnace adopts Si
3n
4in conjunction with SiC brick or Sialon in conjunction with SiC brick.Si
3n
4possess the excellent performances such as hot strength is high, wear-resisting in conjunction with SiC brick and Sialon in conjunction with SiC brick but price is high, limit its applying at blast furnace.
Kyanite, andaluzite, sillimanite three kinds of mineral are referred to as " three stone " 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, are thus at high temperature converted into the temperature of mullite, time, speed and volume effect all not identical, are converted into the process of mullite, form, crystallization direction 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 about 1400 DEG C time, and conversion rates is medium, and volume kept stable after changing, 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 at service temperatures, all there is 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, improving the performance of traditional refractory materials, to meet the particular requirement of hot industry to refractory materials.Zhu Liming etc. by research sillimanite and andaluzite to Al
2o
3one SiO
2be the impact of product properties, draw: the Al adding 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.The Low Creep High Alumina Bricks that Wang Xinquan etc. are raw material development and production with special grade bauxite grog, Brown Alundum, high alumina corundum, mullite, sillimanite, andaluzite and clay etc. has desirable weave construction, the own all mullitizations of andaluzite particle in sample, part sillimanite changes mullite into, and mullite is mutually in staggered network structure.
China's " three stone " Mineral resources are quite abundant, find " three stone " mineral deposit (point) nearly hundred places at 25 provinces, municipalities and autonomous regions at present.But " three stone " Mineral resources totally utilize level lower at present, cause the waste of " three stone " Mineral resources to a certain extent.Therefore, base oneself upon china natural resources advantage, strengthen the Application Areas research of " three stone ", " three stone " product innovation of effort 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, and the polysilicon market as main raw material also constantly expands thereupon.But polysilicon can use after needing to cut into silicon chip.At cutting process because cutter damages enter cutting slurry by there being the crystalline silicon of 50%-52% to become silicon powder, cause cutting efficiency to reduce, final cutting slip lost efficacy and became slug, caused the wasting of resources and environmental pollution, brought huge pressure to enterprise.Generally adopt at present silicon carbide as cutting abrasive material, therefore cut in slug main containing 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 in cutting waste material how is recycled cost-effectively and silicon carbide is also current problem demanding prompt solution.
Summary of the invention
The object of this invention is to provide a kind of good thermal shock, anti-CO and alkali vapours attack is strong, creep-resistant property is excellent, the preparation method of the material of high volume good stability and 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 promote the exploitation 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 the match used of a kind of blast furnace stack middle and upper part grand in conjunction with andaluzite/sillimanite/SiC composite refractory, by weight percentage, raw material consists of: 5-15% granularity is the andaluzite of 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, be 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%, and it is 0.5-3% that content of MgO is less than 1%, PEG content; The granularity of described aluminium powder is 200 orders, Al>=97% in aluminium powder.
The grand preparation method in conjunction with andaluzite/sillimanite/SiC composite refractory of match that blast furnace stack middle and upper part is used, described preparation method comprises the following steps:
A. take various raw material by described proportioning, powder part is carried out premix, do time as 30-60min in advance, it is 1-0mm sillimanite that described powder part comprises granularity, α-Al
2o
3powder, polycrystalline silicon wastes, aluminium powder.
B. andaluzite, 3-1mm sillimanite that granularity is 5-3mm is first added, add 2/3 of the total add-on of the bonding agent formed by dextrin, resol prepared in advance again, mixing 1-5min, then the powder and remaining 1/3 bonding agent that obtain through premix in step a is added, remix 5-10min.
C. the mixture obtained by step b is pressed into firebrick billet through friction press or vibration pressure machine.
D. the firebrick billet of forming is put into moisture eliminator 110 ± 10 DEG C of dry 24-48h, control moisture content below 0.5%.
E. dried adobe is imported muffle combustion gas nitrogenize shuttle kiln, burn till in 1200-1600 DEG C of nitrogen atmosphere, final obtained match is grand in conjunction with andaluzite/sillimanite/SiC composite refractory brick.
Compared with prior art, feature of the present invention and positively effect:
1. the present invention utilizes Si, it is grand in conjunction with andaluzite/sillimanite/SiC composite refractory that Al metal transfer phase technique has prepared match, production technique is simple, identical in conjunction with SiC refractory material production technique with traditional Si alon, special requirement is not proposed to the production unit of refractory materials, to enrich with reserves in China and the andaluzite urgently developed and sillimanite are raw material simultaneously, not only increase the heat-shock resistance of material, creep-resistant property, the ability of anti-CO and alkali vapours attack, also preparation cost is greatly reduced, product of the present invention is made to have 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 at service temperatures, unconverted andaluzite and sillimanite is all had to decompose the expansion produced, thus make goods inside produce certain stress, 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, goods are made to have comparatively ideal weave construction: andaluzite particle and sillimanite portions turn are mullite, pin rod-like mullite is woven into network structure, makes material possess the ability of superior heat-shock resistance, creep resistance, high volume stability and stronger anti-CO and alkali vapours attack.
3. grand the combination in conjunction with Sialon in andaluzite/sillimanite/SiC composite refractory of match that prepared by the present invention is Si-Al-O-N sosoloid mutually, its solid solubility can change within the specific limits, does not affect the grand acquisition in conjunction with andaluzite/sillimanite/SiC composite refractory of last match when feed composition slightly changes.Therefore this technique is lower to ingredient requirement, is applicable to industrialization promotion.
4. the match prepared of the present invention is grand possesses excellent physical performance index in conjunction with andaluzite/sillimanite/SiC composite refractory.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 higher than 1700 DEG C, there is the ability of good heat-shock resistance, creep resistance and stronger anti-CO, alkali steam corrosion.
5. product of the present invention given full play to andaluzite and sillimanite good thermal shock, anti-CO and alkali steam corrosion ability strong, the features such as mullite can be changed at different temperatures, and Appropriate application abundance, cheap polycrystalline silicon wastes produces Sialon in conjunction with phase, improve the hot strength of material, oxidation-resistance, high temperature abrasion resistance, product is not only made to possess high performance-price ratio, also under the prerequisite not being separated SiC and Si, achieve the utilization of polycrystalline silicon wastes, decrease 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 the refractory materials kind reducing the use of blast furnace stack middle and upper part, reduces the workload that body of heater is built by laying bricks or stones, improve the globality of body of heater, improve the work-ing life of blast furnace.
Embodiment
Embodiment 1: the match used of a kind of blast furnace middle and upper part is grand in conjunction with andaluzite/sillimanite/SiC composite refractory and preparation method, by weight percentage, raw material consists of: 8% granularity is the andaluzite of 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 material by described proportioning, powder part is carried out premix, do time as 30-60min in advance, it is 1-0mm sillimanite that described powder part comprises granularity, 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 2/3 of the total add-on of the bonding agent formed by dextrin, resol prepared in advance again, mixing 1-5min, then the powder and remaining 1/3 bonding agent that obtain through premix in step a is added, remix 5-10min.
C. the mixture obtained by step b is pressed into firebrick billet through friction press or vibration pressure machine.
D. the firebrick billet of forming is put into moisture eliminator 110 DEG C of dry 48h, control moisture content below 0.5%.
E. dried adobe is imported muffle combustion gas nitrogenize shuttle kiln, burn till in 1450 DEG C of nitrogen atmospheres, final obtained match is grand in conjunction with andaluzite/sillimanite/SiC composite refractory brick.
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 of good heat-shock resistance, creep resistance and stronger anti-CO and alkali vapours attack.
Embodiment 2: production technique is identical with embodiment 1, and difference is:
By weight percentage, raw material consists of: 8% granularity is the andaluzite of 5-3mm, and 37% granularity is the sillimanite of 3-1mm, and 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 of good heat-shock resistance, creep resistance and stronger anti-CO and alkali vapours attack.
Claims (2)
1. a match is grand in conjunction with andaluzite/sillimanite/SiC refractory material, it is characterized in that: by weight percentage, raw material consists of: 5-15% granularity is the andaluzite of 5-3mm, and 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 are 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%; The granularity of described polycrystalline silicon wastes is discrete distribution, be between 1 μm and 240 μm, mean particle size is 20 μm ± 10 μm, 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%, and it is 0.5-3% that content of MgO is less than 1%, PEG content; The granularity of described aluminium powder is 200 orders, Al>=97% in aluminium powder.
2. the grand preparation method in conjunction with andaluzite/sillimanite/SiC refractory material of match according to claim 1, is characterized in that:
A. take various raw material by described proportioning, powder part is carried out premix, do time as 30-60min in advance, it is 1-0mm sillimanite that described powder part comprises granularity, α-Al
2o
3powder, polycrystalline silicon wastes, aluminium powder;
B. andaluzite, 3-1mm sillimanite that granularity is 5-3mm is first added, add 2/3 of the total add-on of the bonding agent formed by dextrin, resol prepared in advance again, mixing 1-5min, then the powder and remaining 1/3 bonding agent that obtain through premix in step a is added, remix 5-10min;
C. the mixture obtained by step b is pressed into firebrick billet through friction press or vibration pressure machine;
D. the firebrick billet of forming is put into moisture eliminator 110 ± 10 DEG C of dry 24-48h, control moisture content below 0.5%;
E. dried adobe is imported muffle combustion gas nitrogenize shuttle kiln, burn till in 1200-1600 DEG C of nitrogen atmosphere, final obtained match is grand in conjunction with andaluzite-sillimanite-SiC composite refractory brick.
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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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|---|---|---|---|
| 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 true CN103979988B (en) | 2015-04-22 |
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|---|---|---|---|---|
| CN106220194A (en) * | 2016-07-11 | 2016-12-14 | 雷春生 | A kind of preparation method of low creep anti-thermal shock burner block |
| 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 |
| CN115286404B (en) * | 2022-08-23 | 2023-01-06 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101450866A (en) * | 2007-12-04 | 2009-06-10 | 上海宝钢工业检测公司 | Abrasion resistant steel fiber reinforcement pouring precast block for coke dry quenching oven |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4838619B2 (en) * | 2006-04-04 | 2011-12-14 | 黒崎播磨株式会社 | Alumina-silica brick for CDQ |
-
2014
- 2014-05-27 CN CN201410228451.0A patent/CN103979988B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101450866A (en) * | 2007-12-04 | 2009-06-10 | 上海宝钢工业检测公司 | Abrasion resistant steel fiber reinforcement pouring precast block for coke dry quenching oven |
| 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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