CN1303036C - Process for preparing high strength corundum refractory material by low temperature sintering - Google Patents
Process for preparing high strength corundum refractory material by low temperature sintering Download PDFInfo
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- CN1303036C CN1303036C CNB2004100605157A CN200410060515A CN1303036C CN 1303036 C CN1303036 C CN 1303036C CN B2004100605157 A CNB2004100605157 A CN B2004100605157A CN 200410060515 A CN200410060515 A CN 200410060515A CN 1303036 C CN1303036 C CN 1303036C
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Abstract
The present invention provides a method for preparing a high-strength corundum fire resisting material by a low-temperature sintering process. In the method for preparing a high-strength corundum fire resisting material by a low-temperature sintering process, corundum raw materials which are particularly electric melting white corundum aggregate and powder are used as main raw materials, silicon ash (a smoke waste gas recovery object in an iron alloy factory) having the advantages of small granularity, large activity, rich good supply and low price is added on the basis of corundum multi-stage granule mixing materials and is used as a sintering aid, and after a mixing process and a forming process, the high-strength corundum fire resisting material is prepared by the sintering process under low temperature (1300 DEG C to 1550 DEG C). The method for preparing a high-strength corundum fire resisting material by a low-temperature sintering process can produce the product of the good-quality corundum fire resisting material and can also considerably save energy source and reduce production cost, the high-strength corundum fire resisting material has the advantages of low sintering temperature, large strength, high temperature resistance and corrosion resistance, and the high-strength corundum fire resisting material can be used as the advanced fire resisting materials and the ceramic wares of the high temperature furnaces of industries, such as metallurgy, construction materials, chemical industries, ceramics, etc.
Description
Technical field:
The invention belongs to pottery, refractory materials preparing technical field, being specifically related to a kind of is the preparation method of the low-temperature sintering high strength refractory corundum material of main raw material by fused white corundum aggregate and powder.
Background technology:
Corundum refractory has excellent mechanical property, and it is high temperature resistant, corrosion-resistant, wear-resistant, be develop the earliest, the present bigger a kind of high grade refractory of turnout, be mainly used in field high temperature kiln key position liners such as iron and steel, chemical industry, pottery, machinery, yet the sintering temperature height of corundum based refractory materials, usually more than 1600 ℃, production cost is high, has influenced the widespread use of this material to a certain extent.
In order to reduce the firing temperature of corundum refractory, the method that adopts mainly contains usually:
(1) adds boric acid or B
2O
3Method: after 1550 ℃ of calcinings, make Na
2O generates Sodium Tetraborate and volatilizees, and adds B
2O
3To SiO
2Content aluminum oxide refining effect high and that weave construction is perfect is very effective, but because aluminum oxide forms the coarse-grain structure, therefore density, mechanical property and the dielectric properties of special refractories is all decreased;
(2) MgCl
2Not only can remove the Na in the aluminum oxide
2O, it still burns till the desired crystal formation of corundum ceramic goods and transforms conditioning agent, and does not need to adopt the auxiliary process measure.This method be widely used in produce chemical pure, under vacuum fine and close extraordinary corundum ceramic goods, the corundum grog of Sheng Chaning in this way can the production chemical ingredients, mechanical property and the extra high corundum products of density, sintering temperature is 1500-1620 ℃.Add appropriate MgO and also can promote the sintering of corundum based refractory materials, and improve the intensity of burning till the back material.
(3) if add TiO
2Or MnCO
3Though the corundum refractory calcining temperature can be reduced to 1600 ℃, these two kinds of additives can both make the crystal grain growth grow up, and significantly reduce the physical strength of material, make material painted simultaneously.
(4) add Cr
2O
3Or ZrO
21600 ℃ of corundum based refractory materials burn till after, have excellent high-temperature intensity and thermal shock resistance.
According to putting down in writing in the CSTAD, the heavy oil pressurized-gasification furnace corundum products project of Refractory Material Factory, Xinxiang City's evaluation in 1993 is characterized in adding an amount of alumina powder in batching, and adopts phosphate binders, burns till at 1550-1610 ℃.The high-purity corundum brick of Luoyang Institute of Refractories Research's evaluation in 1992, be characterized in adopting showing under two kinds of high temperature that different electric smelting and the alundums that burn till contraction are main raw material, and add part active oxidation aluminium powder, multiple stage material compounding, two-sided extrusion forming, high temperature are burnt till and are made.
Application number is 00123761.6 patent, a kind of high-purity low silicon and low iron corundum products is disclosed, being characterized in removing in batching fused corundom, sintered alumina fine powder and wedding agent adds into micro-calcareous material as sintering aid, improved the sintering situation of brick, make brick burn till the good sintering of realization under the temperature low, the high-purity corundum brick cold crushing strength of making is about 110MPa.
Application number is 99123977.6 patent, adds the kaolin fine powder relatively largely in matrix, thereby prepares corundum-mullite product.
Application number is the patent of 88104671.X, be characterized in sintered sheet corundum crystalline particle moulding in prefabricated model of all having cleavage surface by numerous, then through 1500 ℃ of sintering, make and assemble mutually between the particle and combine, its combination makes that the cleavage surface of these accumulative plate crystal granules is parallel to each other substantially, thereby prepares high flexural strength sintered alumina article.
The problem that the method for putting down in writing in the above-mentioned document for preparing corundum refractory exists is, firing temperature is higher, and energy consumption is big, and the cost height has influenced the production of corundum refractory and being extensive use of in hot industry thereof to a certain extent.
Summary of the invention:
The purpose of this invention is to provide a kind of silicon ash that utilizes cheapness as sintering aid, prepare the method for high strength refractory corundum material at a lower temperature,, cut down the consumption of energy and preparation cost, be beneficial to industry manufacturing to reduce firing temperature.
Principle of the present invention is to add the proper amount of silicon ash in the corundum raw material, utilizes the short nodulizing of the higher silicon ash of sintering activity under the high temperature, makes the corundum material Fast Sintering, thereby obtains low sintering high-strength corundum material.If silicon ash add-on very little, in temperature of the present invention, material does not reach good sintering state, and intensity is lower.If but silicon ash add-on is excessive, the interior mullite synthesizing of material is mutually too much in the sintering process, and volumetric expansion is bigger, influences the performance of product.Therefore, the add-on of silicon ash should be suitable.
Realize that the object of the invention technical scheme is:
The preparation method of low-temperature sintering high strength refractory corundum material comprises that mainly raw material mixes, adds wedding agent, mixing, shaping and drying, technological process such as burns till, and is characterized in that:
A. with electric smelting or alundum raw material crushing or be ground into 3-1mm, 1-0.088mm, the particle of three kinds of granularities below the 0.088mm;
B. make sintering aid with silicon ash or monox nanometer powder, mix in the corundum in granules material below massfraction 1-9% (adding) ratio and the 0.088mm, as the matrix material;
C. the corundum in granules material with 3-1mm, 1-0.088mm mixes;
D. add wedding agent in the c compound, after mixing, add the matrix material that b obtains, remix is even, makes pug
E. the pug that d is made is put into pressing machine, is pressed into base substrate under 70-200MPa pressure, and drying was burnt till 2-8 hour under 1300-1550 ℃ of temperature then, and cooling is come out of the stove, and promptly makes product.
Among the above-mentioned preparation method, 3-1mm, 1-0.088mm, the following three kinds of different corundum raw material ratio of mixture of 0.088mm are 40-50%: 10-20%: 30-40%, are preferably 45: 15: 40; The add-on of wedding agent is the 3-15% of corundum raw material.
Among the above-mentioned preparation method, used corundum raw material is a kind of in fused white corundum, plate diamond spar, brown corundum, grey corundum, bauxite corundum, the alundum; Wedding agent is one or more in industry sulphate pulp waste liquid, polyvinyl alcohol, dextrin, the xylogen.
With the corundum material that the inventive method makes, thing phase composite: corundum 〉=98%, physical and chemical performance: Al
2O
3〉=90%, volume density 2.8-3.2g/cm
3, apparent porosity≤25%, strength at normal temperature 〉=20MPa, cold crushing strength 〉=80MPa.
Compared with prior art, the invention has the advantages that:
1, adopts the silicon ash as sintering aid, reduced the firing temperature of material, reduced preparation cost.
2, Zhi Bei strength of materials height, the work-ing life that helps improving material.
3, silicon ash source is abundant, cheap, and short nodulizing is obvious.
Embodiment
Embodiment 1:
The employed main raw material of present embodiment is:
(1) fused white corundum: chemical ingredients (massfraction) is Al
2O
3〉=98%, granularity is following three kinds of 3-1mm, 1-0.088mm, 0.088mm;
(2) silicon ash: select SiO for use
2〉=91%.
Raw material of the present invention and silicon ash proportioning are as shown in the table:
| Raw material | Fused white corundum | The silicon ash | ||
| Grain size proportion (weight fraction %) | 3-1mm 45 | 1-0.088mm 15 | ＜0.088mm 40 | 0.1μm 4 |
Take by weighing various fused white corundum raw materials in ratio shown in the last table, wherein adding the silicon ash is 4%.Earlier the following fused white corundum particulate material of 0.088mm and silicon ash are mixed the matrix material; Again with 3-1mm, the Preblend of 1-0.088mm particulate, and add 3% polyvinyl alcohol wedding agent and put into mixer and mix, add the matrix material at last and in mixer, mix 5 minutes to evenly promptly making pug; Pug is put into pressing machine go out 25 * 25 * 125mm base substrate at the 80MPa forming under the pressure; Base substrate was 110 ℃ of dryings 4 hours; 1350 ℃ * 6h burns till in electric furnace then, and cooling is come out of the stove, and makes corundum material.
The corundum material performance that makes is as follows: Al
2O
3〉=90%, volume density 2.9g/cm
3, apparent porosity 25%, strength at normal temperature 33.4MPa, cold crushing strength 105MPa.
Embodiment 2:
The employing fused brown corundum is a particulate material, and proportioning raw materials and preparation technology go out 25 * 25 * 125mm base substrate with embodiment 1 at the 120MPa forming under the pressure; Base substrate was 110 ℃ of dryings 4 hours; In electric furnace, burn till 1550 ℃ * 6h.The corundum material performance that makes is as follows: principal crystalline phase is the corundum phase, Al
2O
3〉=90%, volume density 3.0g/cm
3, apparent porosity 23%, strength at normal temperature 35MPa, the material mineral facies consist of more purified corundum phase.
Embodiment 3:
Add 9% silicon ash in batching, wedding agent adopts lignosulfite, and other raw materials and proportioning and preparation technology go out 25 * 25 * 125mm base substrate with embodiment 1 at the 120MPa forming under the pressure; Base substrate was 110 ℃ of dryings 4 hours; In electric furnace, burn till 1350 ℃ * 6h.The corundum material performance that makes is as follows: principal crystalline phase is the corundum phase, Al
2O
3〉=90%, volume density 3.1g/cm
3, apparent porosity 19%, strength at normal temperature 45MPa, the material mineral facies consist of corundum mutually with the trace mullite mutually.
Claims (5)
1, a kind of preparation method of low-temperature sintering high strength refractory corundum material comprises that mainly raw material mixes, adds wedding agent, moulding, drying, firing process process, is characterized in that:
A. with electric smelting or alundum raw material crushing or be ground into 3-1mm, 1-0.088mm, the particle of three kinds of granularities below the 0.088mm, its ratio of mixture is 40-50%: 10-20%: 30-40%;
B. make sintering aid with silicon ash or monox nanometer powder, mix in massfraction 1-9% ratio and the corundum in granules material below the 0.088mm, as the matrix material;
C. the corundum in granules material with 3-1mm, 1-0.088mm mixes;
D. in the compound of c, add wedding agent and mix, add the matrix material of b again, mix, make pug;
E. the pug that d is made is put into pressing machine, is pressed into base substrate under 70-200MPa pressure, and drying was burnt till 2-8 hour under 1300-1550 ℃ of temperature then, and cooling is come out of the stove, and promptly makes product.
2, according to the preparation method of the described low-temperature sintering high strength refractory corundum material of claim 1, it is characterized in that: the ratio of mixture of 3-1mm, 1-0.088mm, the following three kinds of different corundum raw materials of 0.088mm is 45%: 15%: 40%.
3, according to the preparation method of the described low-temperature sintering high strength refractory corundum material of claim 1, it is characterized in that: the add-on of wedding agent is the 3-15% of corundum raw material.
4, according to the preparation method of the described low-temperature sintering high strength refractory corundum material of claim 1, it is characterized in that: said corundum raw material is a kind of in fused white corundum, plate diamond spar, brown corundum, grey corundum, bauxite corundum, the alundum.
5, according to the preparation method of the described low-temperature sintering high strength refractory corundum material of claim 1, it is characterized in that: said wedding agent is one or more in lignosulfite, polyvinyl alcohol, dextrin, the xylogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100605157A CN1303036C (en) | 2004-09-15 | 2004-09-15 | Process for preparing high strength corundum refractory material by low temperature sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100605157A CN1303036C (en) | 2004-09-15 | 2004-09-15 | Process for preparing high strength corundum refractory material by low temperature sintering |
Publications (2)
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|---|---|
| CN1587189A CN1587189A (en) | 2005-03-02 |
| CN1303036C true CN1303036C (en) | 2007-03-07 |
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Families Citing this family (11)
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|---|---|---|---|---|
| CN100436369C (en) * | 2005-03-29 | 2008-11-26 | 郑州大学 | Method for preparing corundum bricks composite with Nano alpha-Al2O3 |
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| CN106220203B (en) * | 2016-08-06 | 2019-03-26 | 山东铭特陶瓷材料有限公司 | The preparation method of wear-resistant ceramic load bearing board |
| CN106588098B (en) * | 2017-01-09 | 2019-06-25 | 武汉科技大学 | A kind of diffusion-type corundum-spinel air brick and preparation method thereof |
| CN106946589B (en) * | 2017-03-24 | 2019-06-21 | 山东磐石刚玉有限公司 | The technique and the technique device therefor of Brown Alundum plating zirconium oxide |
| CN114105676B (en) * | 2020-12-31 | 2023-08-15 | 郑州轻工业大学 | Corundum micro-nano Kong Jue heat-insulating refractory material and preparation method thereof |
| CN113149618A (en) * | 2021-05-08 | 2021-07-23 | 湖南聚福精密陶瓷有限责任公司 | Ceramic burning bearing plate and processing technology thereof |
| CN115477533A (en) * | 2022-10-17 | 2022-12-16 | 中冶赛迪工程技术股份有限公司 | Nano ZrO 2 Toughened high-alumina refractory brick and preparation method and application thereof |
| CN116589265A (en) * | 2023-04-15 | 2023-08-15 | 河南铠甲节能科技有限公司 | High-temperature refractory module with ultrahigh compressive strength and ultralow heat conductivity coefficient |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123860A (en) * | 1981-01-22 | 1982-08-02 | Shinagawa Refractories Co | Alumina carbon refractories |
| US5589426A (en) * | 1992-07-14 | 1996-12-31 | Taikorozai Co., Ltd. | Monolithic refractories |
| JPH11171657A (en) * | 1997-12-12 | 1999-06-29 | Hazuru Dolomite Kogyo Kk | Castable refractory |
| CN1313261A (en) * | 2001-04-27 | 2001-09-19 | 项新惠 | Refractory for cupola furnace |
| CN1398823A (en) * | 2001-07-24 | 2003-02-26 | 杨晓芳 | High-strength wear-resistant cast material of compact electrically molten corundum |
-
2004
- 2004-09-15 CN CNB2004100605157A patent/CN1303036C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57123860A (en) * | 1981-01-22 | 1982-08-02 | Shinagawa Refractories Co | Alumina carbon refractories |
| US5589426A (en) * | 1992-07-14 | 1996-12-31 | Taikorozai Co., Ltd. | Monolithic refractories |
| JPH11171657A (en) * | 1997-12-12 | 1999-06-29 | Hazuru Dolomite Kogyo Kk | Castable refractory |
| CN1313261A (en) * | 2001-04-27 | 2001-09-19 | 项新惠 | Refractory for cupola furnace |
| CN1398823A (en) * | 2001-07-24 | 2003-02-26 | 杨晓芳 | High-strength wear-resistant cast material of compact electrically molten corundum |
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|---|---|
| CN1587189A (en) | 2005-03-02 |
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