CN1807352A - Higly oxidized zirconia refractory preparation method - Google Patents
Higly oxidized zirconia refractory preparation method Download PDFInfo
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- CN1807352A CN1807352A CN 200510044209 CN200510044209A CN1807352A CN 1807352 A CN1807352 A CN 1807352A CN 200510044209 CN200510044209 CN 200510044209 CN 200510044209 A CN200510044209 A CN 200510044209A CN 1807352 A CN1807352 A CN 1807352A
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- zirconia refractory
- oxidized zirconia
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/42—Details of construction of furnace walls, e.g. to prevent corrosion; Use of materials for furnace walls
- C03B5/43—Use of materials for furnace walls, e.g. fire-bricks
Abstract
The invention relates to a preparation method for improved high-zircite refractory material. Wherein, selecting the material as 88-98% crushed material with monocrystal ZrO2 as main component and alumina powder; ball grinding the material to its size D50 up to 1-10mu m; spraying, drying, and granulating; with equal static pressure forming method, controlling strictly the temperature between the phase transformation temperature of monoclinic crystal and regular crystal. This invention can obtain quality-super sintered refractory material with well corrosion resistance to prolong the up-to-standard rate of glass production and the equipment lifetime, and can also be used in other fields.
Description
Technical field
The present invention relates to a kind of preparation method of improved Higly oxidized zirconia refractory, be technical field of refractory materials.
Background technology
Glass furnace in the past roughly is divided into sintered refractory and fused refractory with refractory materials.Sintered refractory because of void content generally about 10%, easy bubbling and aggregate break away from when being used for the glass kiln, and cause glasswork to produce defectives such as bubble, sand grains (aggregate break away from back journey particulate state enters glasswork and the defective that forms), so can not be used for the significant points of glass kiln; General high zirconia sintered refractory, the transformation mutually of oblique crystal and regular crystal takes place in zirconium white between 900 ℃ and 1200 ℃, therefore, add Y
2O
3, stablizer such as MgO and CaO, to avoid it to change mutually, when using the high zirconia sintered refractory that contains stablizer like this on glass furnace, stablizer is dissolved in the glass, and stabilizing zirconia is varied to astable zirconium white, changes mutually to continue to take place, and cause tissue fragile, defectives such as sand grains take place to occur in the glass, and therefore, the high zirconia series sinter refractory materials that contains stablizer can not be used on glass furnace.
Fused refractory is with the refractory materials liquation of electric furnace fusion, abundant homogenizing, waters and casts from sand mold, becomes the refractory product of dense structure, crystallization prosperity behind the cooling curing.The fused refractory that zirconia content is higher, its solidity to corrosion is good, is suitable in the glass melting kiln; Such refractory materials is divided into the Al of zirconia content 33～41% substantially
2O
3-ZrO
2-SiO
2The fused refractory of series and the high zirconia of zirconia content 85～95% series fused refractory.
High zirconia series fused refractory has better solidity to corrosion, and is low to glass feed liquid contaminative, obtained popularization and application in recent years in the high quality glass kiln.But existing high zirconia series refractory materials is because the glassy phase that contains lacks than electric fused zirconium corundum (AZS), speed of cooling difference during casting, have part occur void content high year the colyliform tissue shortcoming, shortcomings such as foaming appear sometimes from this part.
(denomination of invention: zirconium white matter refractory body applicant: in patent Asahi Glass), having with astable fused zirconia and aluminum oxide pulverizing product is the invention of the sintered refractory of raw material at " the special 8-276194 of Yuanping City ".But this method, because of raw material granularity slightly can not produce the high zirconia sintered refractory of compact structure, compare with the Higly oxidized zirconia fused refractory aspect anti-glass metal erosion, also have not enough.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Higly oxidized zirconia sintered refractory, the Higly oxidized zirconia sintered refractory product density height that produces, solidity to corrosion is strong, and is low to the contaminative of glass feed liquid, is fit to be applied on the glass furnace.
The preparation method of Higly oxidized zirconia refractory of the present invention comprises batching, moulding and burns till, and it is characterized in that the ingredients by weight percentage composition is: 88～98% with zirconium white matter fusion cured article monocrystalline series ZrO again
2Be the crushed material of main component and the alumina powder of surplus.Zirconium white matter fusion cured article again is meant the astable zirconium white of electric smelting X950.
In order to guarantee the characteristic of Higly oxidized zirconia refractory, the fusion of zirconium white matter is cured article monocrystalline series ZrO again
2For the chemical weight percentage composition of the crushed material of main component is controlled to be: ZrO
290～98%, SiO
21～9%, surplus is inevitable dirt, as Na
2O, TiO
2Deng.The fusion of zirconium white matter is cured article monocrystalline series ZrO again
2For the crushed material of main component can synthesize voluntarily, also can directly buy, alumina powder has the commercially available prod, directly buys to get final product.
The batch mixes ball milling is reached 1～10 μ m to material particular diameter D50, help obtaining good compactness, do not have be full of cracks, reduce void content,, strengthen solidity to corrosion, reduce contaminative the glass feed liquid below 5%.Ball milling material particular diameter D50 control mode is the smashing fineness phraseology of all knowing on the industry, and the meaning is that 50% grain diameter is within the D50 numerical range.
Ball milling adopts the wet ball-milling mode, adopts polyester rubber ball milling liner, uses the zirconium white composition at the zirconium matter mill ball more than 95%, and grinding medium adopts water more, also can be other grinding medium, as alcohol etc.
Batching behind the ball milling is carried out spraying drying obtain the spraying pellet, particle diameter is suitable less than 0.5mm, according to the moulding requirement, controls dry moisture content, and conventional the requirement gets final product, and no particular requirement is generally below 0.5%.Then pellet is filled in and carries out isostatic pressing in the rubber mold and get work in-process, forming pressure is 110～260MPa.
Work in-process after the moulding are dried under 110～200 ℃ temperature, carry out high temperature again and burn till.For fear of changing the disadvantageous effect that the bigger volume change bring causes between zirconium white oblique crystal and regular crystal crystalline phase, temperature variation will be controlled slowlyer in the crystal phase transition temperature scope, and calcining system control is as follows:
30～1100℃ 0.3～0.5℃/min；
1100～1250℃ 0.1～0.15℃/min；
1250～1600℃ 0.8～1.1℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 0.8～1.1℃/min；
1000～850℃ 0.1～0.15℃/min；
850～30℃ 0.3～0.5℃/min。
Product after burning till is carried out the back arrangement, after handling as cutting, grinding etc., get finished product.It is bigger that product can be done, as being 400 * 600 * 100mm, 500 * 500 * 100mm etc.
Through analysis and research and test of many times, detection prove repeatedly, the technical scheme that the present invention determines can obtain the sintered refractory of superperformance, the homogeneous microstructure densification, flawless, void content is low, and solidity to corrosion is good, and suitable glass furnace uses, be difficult for the defectives such as sand grains in the generation glass, can improve the qualification rate of glass production and the work-ing life of prolongation glass furnace.The refractory products that preparation method of the present invention produces also can be used other suitable occasion and field.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1-5
The preparation method of Higly oxidized zirconia refractory of the present invention, carry out according to following requirement:
(1) the raw materials used chemical weight percentage composition of batching:
The Higly oxidized zirconia fusion is cured article again: ZrO
293.8%, SiO
24.5%, Al
2O
30.95, Na
2O 0.5%.
(α-Al
2O
3) alumina powder: Al
2O
399.30%, Na
2O 0.32%.
(2) ball milling: raw material is prepared burden according to the ingredients by weight percentage composition shown in the table 1, batching is put into ultra tiny wet-type ball mill mix pulverizing, grinding particle size reaches the granularity requirements shown in the table 1.
(3) granulation: the mud that wet ball-milling is obtained is by the sponging granulator granulation of dewatering, and the control of granulation material particle diameter requires to see Table 1, and the pellet pigment control after the granulation gets final product conventional requirement less than 0.5%.
(4) isostatic pressing: the granulation material is filled into carries out isostatic pressing in the rubber mold and make work in-process, forming pressure is 260MPa.
(5) oven dry: with work in-process conventional oven dry in 130～180 ℃ drying oven.
(6) burn till: in zirconic crystalline phase (oblique crystal and regular crystal) transition temperature zone, temperature variation is wanted slowly, and calcining system is:
30～1100℃ 0.5℃/min；
1100～1250℃ 0.1℃/min；
1250～1600℃ 1.1℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 1.1℃/min；
1000～850℃ 0.1℃/min；
850～30℃ 0.5℃/min。
(7) back arrangement: the goods after will burning till cut, grind and make finished product.
Identical among the present invention among the preparation method of NM technology and requirement and conventional refractory materials for conventional prior art, repeats no more.
Embodiment interpretation of result and explanation:
A, raw material pulverizing granularity easily chap after burning till (comparative example No.6) when 1 μ m is following; And when 10 μ m were above, void content is big (comparative example No.7).
B, for Higly oxidized zirconia refractory, α-Al
2O
3When nothing interpolation or addition are above above 10%, easily chap after burning till (comparative example No.8, No.9).
C, Kesternich test are that the sample that is cut into the Nogata shape of 20 * 10 * 120mm is hung in platinum crucible, have measured erosion amount with electric furnace after 1550 ℃ * 4 hours.Erosion material has adopted alkali-free alumina silicate glass.With vernier caliper measurement behind near the erosion amount the slag line and the erosion amount that contains the fused cast refractories of zirconium white 95% compare, calculated anti-corrosion index.The erosion amount (mm) of erosion amount (the mm)/trial target of anti-corrosion index=95% electric capacity brick; Data are big more, and corrosion-resistant property is good more.
Table 1, part embodiment table
| Project | Embodiment | ||||
| The ingredients by weight percentage composition | Embodiment 1 (No.1) | Embodiment 2 (No.2) | Embodiment 3 (No.3) | Embodiment 4 (No.4) | Embodiment 5 (No.5) |
| The high zirconia fusion is cured article again | 98 | 95 | 90 | 95 | 95 |
| α-Al 2O 3 | 2 | 5 | 10 | 5 | 5 |
| Pulverize back particle diameter D50 (μ m) | 2 | 2 | 2 | 4 | 6 |
| Mist projection granulating pellet particle diameter (mm) | ＜0.2 | ＜0.2 | ＜0.2 | ＜0.3 | ＜0.5 |
| Isostatic pressing pressure (MPa) | 260 | 260 | 260 | 260 | 260 |
| Calcining system | See in the literary composition | With embodiment 1 | With embodiment 1 | With embodiment 1 | With embodiment 1 |
| Burn till having or not of back be full of cracks | Do not have | Do not have | Do not have | Do not have | Do not have |
| Void content (%) | 0.4 | 0.3 | 0.2 | 0.5 | 0.7 |
| ZrO 2 | 91.92 | 89.11 | 84.42 | 89.11 | 89.11 |
| Al 2O 3 | 2.92 | 5.87 | 10.23 | 5.87 | 5.87 |
| SiO 2 | 4.41 | 4.28 | 4.05 | 4.28 | 4.28 |
| The solidity to corrosion index | 3 | 2.5 | 1.5 | 2.5 | 2.5 |
Table 2, part test comparative example table
| Project | Comparative example | |||
| The ingredients by weight percentage composition | (No.6) | (No.7) | (No.8) | (No.9) |
| The high zirconia fusion is cured article again | 95 | 95 | 100 | 87 |
| α-Al 2O 3 | 5 | 5 | 0 | 13 |
| Pulverize back particle diameter D50 (μ m) | 1 | 10 | 2 | 2 |
| Mist projection granulating pellet particle diameter (mm) | ＜0.2 | ＜0.5 | ＜0.2 | ＜0.2 |
| Isostatic pressing pressure (MPa) | 260 | 260 | 260 | 260 |
| Calcining system | With embodiment 1 | With embodiment 1 | With embodiment 1 | With embodiment 1 |
| Burn till having or not of back be full of cracks | Have | Have | Have | Have |
| Void content (%) | 0.2 | 2.3 | 3.5 | 0.5 |
| ZrO 2 | 89.11 | 89.11 | 93.8 | 81.61 |
| Al 2O 3 | 5.87 | 5.87 | 0.95 | 13.02 |
| SiO 2 | 4.28 | 4.28 | 4.5 | 3.91 |
| The solidity to corrosion index | 2.5 | 1 | 0.9 | 0.7 |
Embodiment 6
The preparation method of Higly oxidized zirconia refractory of the present invention, carry out according to following requirement:
(1) the raw materials used chemical weight percentage composition of batching:
The Higly oxidized zirconia fusion is cured article again: ZrO
294.8%, SiO
23.7%, Al
2O
30.93%, Na
2O 0.5%.
(α-Al
2O
3) alumina powder: Al
2O
399.40%, Na
2O 0.30%.
(2) ball milling: with raw material according to 93% with zirconium white matter fusion cured article monocrystalline series ZrO again
2Prepare burden for the crushed material of main component and the alumina powder of surplus, batching is put into ultra tiny wet-type ball mill mix pulverizing, grinding particle size control D50 reaches 3.5 μ m.
(3) granulation: the mud that wet ball-milling is obtained is by the sponging granulator granulation of dewatering, and granulation material particle diameter is controlled less than 0.4mm, and the pellet pigment after the granulation are controlled to be 0.4%.
(4) isostatic pressing: the granulation material is filled into carries out isostatic pressing in the rubber mold and make work in-process, forming pressure is 200MPa.
(5) oven dry: work in-process are dried in 110～150 ℃ drying oven.
(6) calcining system is:
30～1100℃ 0.35℃/min；
1100～1250℃ 0.12℃/min；
1250～1600℃ 1℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 0.9℃/min；
1000～850℃ 0.1℃/min；
850～30℃ 0.3℃/min。
(7) back arrangement: the goods after will burning till cut, grind and make finished product.
Embodiment 7
The preparation method of Higly oxidized zirconia refractory of the present invention, carry out according to following requirement:
(1) the raw materials used chemical weight percentage composition of batching:
The Higly oxidized zirconia fusion is cured article again: ZrO
293.2%, SiO
24.8%, Al
2O
30.94%, Na
2O 0.5%.
(α-Al
2O
3) alumina powder: Al
2O
399.20%, Na
2O 0.42%.
(2) ball milling: with raw material according to 96% with zirconium white matter fusion cured article monocrystalline series ZrO again
2Prepare burden for the crushed material of main component and the alumina powder of surplus, batching is put into ultra tiny wet-type ball mill mix pulverizing, grinding particle size control D50 reaches 5.5 μ m.
(3) granulation: the mud that wet ball-milling is obtained is by the sponging granulator granulation of dewatering, and granulation material particle diameter is controlled less than 0.45mm, and the pellet pigment after the granulation are controlled to be 0.5%.
(4) isostatic pressing: the granulation material is filled into carries out isostatic pressing in the rubber mold and make work in-process, forming pressure is 220MPa.
(5) oven dry: work in-process are dried in 140～160 ℃ drying oven.
(6) calcining system is:
30～1100℃ 0.45℃/min；
1100～1250℃ 0.14℃/min；
1250～1600℃ 0.9℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 1.1℃/min；
1000～850℃ 0.13℃/min；
850～30℃ 0.4℃/min。
(7) back arrangement: the goods after will burning till cut, grind and make finished product.
Embodiment 8
The preparation method of Higly oxidized zirconia refractory of the present invention, carry out according to following requirement:
(1) the raw materials used chemical weight percentage composition of batching:
The Higly oxidized zirconia fusion is cured article again: ZrO
291.8%, SiO
26.4%, Al
2O
30.95%, Na
2O 0.4%.
(α-Al
2O
3) alumina powder: Al
2O
399.35%, Na
2O 0.32%.
(2) ball milling: with raw material according to 89% with zirconium white matter fusion cured article monocrystalline series ZrO again
2Prepare burden for the crushed material of main component and the alumina powder of surplus, batching is put into ultra tiny wet-type ball mill mix pulverizing, grinding particle size control D50 reaches 5 μ m.
(3) granulation: the mud that wet ball-milling is obtained is by the sponging granulator granulation of dewatering, and granulation material particle diameter is controlled less than 0.3mm, and the pellet pigment after the granulation are controlled to be 0.35%.
(4) isostatic pressing: the granulation material is filled into carries out isostatic pressing in the rubber mold and make work in-process, forming pressure is 180MPa.
(5) oven dry: work in-process are dried in 120～160 ℃ drying oven.
(6) calcining system is:
30～1100℃ 0.5℃/min；
1100～1250℃ 0.13℃/min；
1250～1600℃ 1.1℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 0.9℃/min；
1000～850℃ 0.12℃/min；
850～30℃ 0.4℃/min。
(7) back arrangement: the goods after will burning till cut, grind and make finished product.
Claims (8)
1, a kind of preparation method of Higly oxidized zirconia refractory comprises batching, moulding and burns till, and it is characterized in that the ingredients by weight percentage composition is: 88～98% with zirconium white matter fusion cured article monocrystalline series ZrO again
2Be the crushed material of main component and the alumina powder of surplus.
2, the preparation method of Higly oxidized zirconia refractory according to claim 1 is characterized in that zirconium white matter fusion cured article monocrystalline series ZrO again
2For the weight percent of the crushed material of main component consists of:
ZrO
2 90～98％、SiO
2 1～9％。
3, the preparation method of Higly oxidized zirconia refractory according to claim 1 is characterized in that the batch mixes ball milling is reached 1～10 μ m to particle diameter D50.
4, the preparation method of Higly oxidized zirconia refractory according to claim 3 is characterized in that the calcining system of the refractory materials after the moulding is:
30～1100℃ 0.3～0.5℃/min；
1100～1250℃ 0.1～0.15℃/min；
1250～1600℃ 0.8～1.1℃/min；
1600 ℃ of insulation 380min;
1600～1000℃ 0.8～1.1℃/min；
1000～850℃ 0.1～0.15℃/min；
850～30℃ 0.3～0.5℃/min。
5, the preparation method of Higly oxidized zirconia refractory according to claim 4 is characterized in that forming method adopts isostatic pressing method.
6, the preparation method of Higly oxidized zirconia refractory according to claim 5 is characterized in that the spraying drying pellet after the used powder of isostatic pressing is for the batching ball milling.
7, the preparation method of Higly oxidized zirconia refractory according to claim 6, the particle diameter that it is characterized in that the spraying drying pellet is less than 0.5mm.
8, the preparation method of Higly oxidized zirconia refractory according to claim 7, the forming pressure that it is characterized in that isostatic pressing is 100～260MPa.
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| CN101851107A (en) * | 2010-05-06 | 2010-10-06 | 广州市石基耐火材料厂 | Compact zircon brick with low alkali content, hole fusion rate and stress and manufacturing method thereof |
| CN101475392B (en) * | 2009-01-21 | 2011-08-03 | 中国化工供销太原贵金属有限公司 | Method for manufacturing noble metal smelting vessel |
| CN102167604A (en) * | 2010-12-31 | 2011-08-31 | 山东省药用玻璃股份有限公司 | Spray repair agent for hot repair of glass furnace |
| CN102718511A (en) * | 2012-06-27 | 2012-10-10 | 巨石集团有限公司 | Semi-lightweight high-zirconium refractory material |
| CN104364205A (en) * | 2012-03-12 | 2015-02-18 | 康宁股份有限公司 | Methods for reducing zirconia defects in glass sheets |
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| CN101851107A (en) * | 2010-05-06 | 2010-10-06 | 广州市石基耐火材料厂 | Compact zircon brick with low alkali content, hole fusion rate and stress and manufacturing method thereof |
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| CN102167604A (en) * | 2010-12-31 | 2011-08-31 | 山东省药用玻璃股份有限公司 | Spray repair agent for hot repair of glass furnace |
| CN102167604B (en) * | 2010-12-31 | 2013-04-24 | 山东省药用玻璃股份有限公司 | Spray repair agent for hot repair of glass furnace |
| CN104364205A (en) * | 2012-03-12 | 2015-02-18 | 康宁股份有限公司 | Methods for reducing zirconia defects in glass sheets |
| CN104364205B (en) * | 2012-03-12 | 2017-04-19 | 康宁股份有限公司 | Methods for reducing zirconia defects in glass sheets |
| CN102718511A (en) * | 2012-06-27 | 2012-10-10 | 巨石集团有限公司 | Semi-lightweight high-zirconium refractory material |
| CN115304375A (en) * | 2022-07-27 | 2022-11-08 | 上海湜清新材料科技有限公司 | Refractory material and preparation process thereof |
| CN115385553A (en) * | 2022-07-28 | 2022-11-25 | 陕西彩虹工业智能科技有限公司 | Microcrystalline glass's smelting device |
| CN115894018A (en) * | 2023-01-05 | 2023-04-04 | 郑州方铭高温陶瓷新材料有限公司 | Glass kiln material flowing nozzle brick and preparation method thereof |
| CN115894018B (en) * | 2023-01-05 | 2023-09-22 | 郑州方铭高温陶瓷新材料有限公司 | Glass kiln material flow nozzle brick and preparation method thereof |
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