CN101381240B - Method for preparing dichroite heat proof/refractory materials - Google Patents

Method for preparing dichroite heat proof/refractory materials Download PDF

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CN101381240B
CN101381240B CN2008101972077A CN200810197207A CN101381240B CN 101381240 B CN101381240 B CN 101381240B CN 2008101972077 A CN2008101972077 A CN 2008101972077A CN 200810197207 A CN200810197207 A CN 200810197207A CN 101381240 B CN101381240 B CN 101381240B
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dichroite
refractory materials
temperature
heat proof
rate
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CN101381240A (en
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何峰
谢俊
程金树
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Wuhan University of Technology WUT
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Abstract

The invention provides a method for preparing a cordierite heat/fire resisting material, namely adding Li-Al-Si system glass powder into the raw materials for preparing the cordierite heat/fire resisting material for ball milling, mixing and processing. The material comprises cordierite crystalline phases and Li-Al-Si system glass crystalline phases. The heat/fire resisting material prepared by the method is not only good in quality, high in performance, but also lower in energy consumption, the firing temperature is 100 to 120 DEG C lower than the prior method on average, the scope of the firing temperature is extended by 80 to 100 DEG C, and the technique is simple, practical and reliable at the same time.

Description

A kind of preparation method of dichroite heat proof/refractory materials
Technical field
The present invention relates to utilize lithium aluminium silicon series system sytull to combine trichroite to prepare the method for heat proof/refractory materials, this material is specially adapted to the preparation of refractoriness less than 1200 ℃ household electrical appliance refractory slab.
Background technology
With the trichroite is the heat-resisting or refractory materials of principal crystalline phase, has very excellent performance.Because light weight, thermal conductivity are low, use temperature is higher relatively and directly be used on the flame front, thereby has reached energy-efficient effect.What also have is used on the higher heat exchanger of cold and hot exchange frequency, like the durable heat pot, and the heat resisting porcelain on the gas furnace, honeycomb kitchen range etc.
The development of cordierite material has the history in more than 100 year.1899, the artificial lens that L.Morozewic at first obtains " Cordierite ", i.e. trichroite.1918, Rankin and Merwin were at research MgO-Al 2O 3-SiO 2In the process of three-part system, synthesized α-type ternary compound, and thought that α-type is identical with L.Morozewicz synthetic trichroite, also identical with natural trichroite.The result of study of nineteen fifty-five Miyashiroetal shows that α-trichroite is a hexagonal system, and β-trichroite possibly be a rhombic system, and the both is different with natural trichroite.On mineralogy, adopt the method for optics and XRD to confirm the difference between α-type and the β-type trichroite, chemical formula Mg 2Al 4Si 5O 18Two polymorphous modification series are arranged: one is hexagonal system, and another is a rhombic system.Afterwards, a large amount of researchists have carried out deep research to the performance of trichroite, and the thermostability that especially trichroite is good and the low coefficient of expansion receive much attention.In the actual production, late 1980s, produced the better low bulk trichroite goods of performance, the trichroite Products Quality improves day by day.The cordierite-quality honeycombed ceramics produced of Corning Incorporated for example, its thermal expansivity (Rt~1000 ℃) is 1.0~1.2 * 10 -6/ ℃, heat-shock resistance reaches 700 ℃.
Comprehensive domestic and international research and preparation about cordierite material can be found, the main raw material of preparation cordierite material, and proportioning is SiO 2-50.15%, Al 2O 3-34.04%, MgO-13.46% burns till more than 3 hours under 1350 ℃ condition, and just can prepare the coefficient of expansion is 1.6-2.4 * 10 -6The trichroite of/℃ (22~800 ℃).
Cordierite ceramic is principal crystalline phase with the cordierite crystal.Cordierite ceramic heat and flame material adopts two kinds of method manufacturings usually, and a kind of is the melten glass crystallization process, and another kind is the powder stock sintering process.
The melten glass crystallization process is that the admixtion that mixes is formed glass through high-temperature fusion, after the moulding, heat-treats and separates out crystal and process cordierite ceramic.This method requires glass smelting even, no bubble, and melt temperature also should be high, reaches more than 1600 ℃.Powder stock sintering rule is worn into fine powder relatively founding under the low temperature after the shrend, carry out sintering after the moulding and make cordierite ceramic, and this method firing temperature can be controlled in below 1450 ℃ and carries out.
Sintering synthetic cordierite material is to be raw material with talcum, kaolin or clay and aluminum oxide etc., and three kinds of raw materials by the suitable proportion mixed preparing, are formed synthesis of dichroite in sintering procedure.For being reduced in the thermal expansivity that forms synthesis of dichroite in the sintering procedure, it is very important that selected suitable raw material are formed, and the proportioning raw materials of synthesis of dichroite all draws according to the trichroite phasor usually, and this compositing area is at SiO 2-Al 2O 3-MgO forms point (2MgO with the trichroite crystallization phases in the phasor 2Al 2O 35SiO 2) be the narrow and small compositing range at center, there is data to show, if its chemical constitution point is respectively near rich MgO side, rich Al 2O 3Some composition points of side, then cordierite ceramic will have lower thermal expansivity.Usually, the proportioning of raw material mixture (by weight) is: the Al of 30%-50% 2O 3, 8%-20% MgO, the SiO of 40%-60% 2, and can carry out certain adjusting.
Because natural trichroite quantity is few, poor performance.Make goods both have certain intensity, arranged long work-ing life again, and develop, generally must adopt the Al of high pure and ultra-fine towards the direction of energy-conservation, high-quality, high yield 2O 3, MgO and SiO 2Powder synthesizes high-purity trichroite, and firing temperature is up to 1350~1440 ℃.Raw materials cost is high, energy consumption is big, thus the bringing a high price of high-purity trichroite synthesis material, thereby can not use widely.Highly purified raw material can synthesize highly purified trichroite, but material purity is high; Impurity is few, and the concentration of the impurity defect that forms in the crystal is low, the diffusion of unfavorable particle; Make solid-phase reaction velocity slow like this, sintered density is poor, has influenced the intensity and the work-ing life of cordierite material.The existence of some impurity in the raw material not only can improve the firing range of trichroite and the work-ing life of having improved cordierite material greatly.
The process characteristic of cordierite goods is generation temperature high (about 1400 ℃) of trichroite, and fusing point low (be decomposed into mullite about 1460 ℃ and contain the magnesium liquid phase) causes the firing range of cordierite goods narrow.Under lower temperature, do not have the trichroite of significant amounts to generate, goods can not sintering; Improve calcining temperature, can cause a large amount of glassy phases to generate, reduce the thermostability of cordierite goods.
The TR of burning till trichroite is narrow, thereby in fact, often adds like Na in the production process 2O, K 2O, CaO, BaO, Fe 2O 3And TiO 2Etc. small amount of impurities, they can reduce temperature of fusion can enlarge melting range again.CaO, Na 2O, K 2O, Fe 2O 3Deng the formation of participation cordierite crystal structure that all can be in various degree, CaO, Fe 2O 3Instead Mg 2+Form substitutional solid solution.Because Ca 2+Ionic radius is greater than Mg 2+, behind the entering trichroite, cause lattice distortion, form the stress room, thereby can reduce synthesis temperature, sintering range is broadened.An amount of Fe 2O 3Can widen firing range, but work as Fe 2O 3Surpass at 0.65% o'clock, then thermal expansivity can sharply rise.TiO 2, BaO, ZrO 2Deng reduction thermal expansivity that all can be in various degree.The introducing of these admixtures can improve and promote the sintering of trichroite, can improve the anti-thermal shock ability of material again.
Aspect the burning till of dichroite heat proof/refractory materials, exist at present: 1. firing temperature is up to 1360~1440 ℃; The TR of 2. burning till trichroite is narrow, the very difficult control of industrial production.
Summary of the invention
Technical problem to be solved by this invention is: prepare the existing problem of dichroite heat proof/refractory materials to above powder stock sintering process; A kind of novel industrialized preparing process that is suitable for is provided, has good quality in the hope of preparing, performance and a dichroite heat proof/refractory materials in work-ing life.
The present invention solves the technical scheme that its technical problem adopts: the lithium aluminium silicon series glass powder of uniting is incorporated in the preparation dichroite heat proof/refractory materials raw material, and with they together ball mill mixing, process.Specifically be the method that adopts following steps:
(1) batching: by weight, take by weighing Al earlier 2O 330~50%, MgO8~20%, SiO 240~60%, mix lithium aluminium silicon series system glass powder by 5~25% of the raw material total mass that takes by weighing at every turn again, get mixture;
(2) ball mill mixing: mixture is put into ball mill, and again by the mixture total mass, the water of adding 35~50%, 1~3% organic additive mixed, grind 10~16 hours, filtered through 300 mesh sieves then, got slip;
(3) prepare base substrate: after slip is carried out spraying drying and granulation, get base substrate through compression moulding;
(4) blank sintering:
Progressively rise to 1240~1360 ℃ by room temperature base substrate carried out sintering, and be incubated 2~5 hours, progressively be cooled to room temperature again, obtain described dichroite heat proof/refractory materials.
The present invention prepares the cordierite material method with existing powder stock sintering process and compares; Its advantage mainly is: through mixing lithium aluminium silicon series system glass powder; Fully utilize the characteristic and advantage of these two kinds of materials of this powder and trichroite; Under relatively low and wide in range temperature, prepare and have good quality and performance and, comprised two main crystalline phases of trichroite crystalline phase and lithium aluminium silicon series system sytull in this material than the heat proof/refractory materials of long life.Utilize the heat proof/refractory materials of present method preparation, its firing temperature on average reduces by 100~120 ℃ than traditional method, and firing range has enlarged 80~100 ℃, so energy consumption decreases.The incorporation of lithium aluminium silicon series system glass powder can be controlled at 5%~25% of each batching total mass.Present method technology is simple, practical, reliable, is suitable for suitability for industrialized production.
Embodiment
Preparation dichroite heat proof/refractory materials method provided by the invention is: the lithium aluminium silicon series glass powder of uniting is incorporated in the preparation dichroite heat proof/refractory materials raw material, and with they together ball mill mixing, process.
Specifically be the method that adopts following steps:
(1) batching: with kaolin, aluminum oxide, talcum powder is main raw material, carries out formula calculation according to the content of various oxide compounds wherein, obtains charger sheet.By weight, take by weighing Al earlier 2O 330~50%, MgO8~20%, SiO 240~60%, mix lithium aluminium silicon series system glass powder by 20% of the raw material total mass that takes by weighing at every turn again, get mixture.
(2) ball mill mixing: mixture is put into ball mill, and again by the mixture total mass, the water of adding 35~50%, 1~3% organic additive mixed, grind 10~16 hours, filtered through 300 mesh sieves then, got slip; Organic additive is Z 150PH or USP Kosher.The addition of organic additive is 1~3% of a mixture total mass.
(3) prepare base substrate: after slip is carried out spraying drying and granulation, get base substrate through compression moulding.
When compression moulding, it is half-dried molded to adopt 1800~2200 tons press to carry out, and utilizes the roller bed type dry kiln that compacted products is carried out drying then.
(4) blank sintering: progressively rise to 1240~1360 ℃ by room temperature base substrate carried out sintering, and be incubated 2~5 hours, progressively be cooled to room temperature again, obtain described dichroite heat proof/refractory materials.
The process that is progressively risen to 1200 ℃ by room temperature is: from room temperature to 500 ℃, temperature rise rate is≤1 ℃/min; 500 ℃ to 1100 ℃, temperature rise rate is 3 ℃/min, and by 1100 ℃ to 1200 ℃, temperature rise rate is 1 ℃/min.
In the process that progressively is cooled to room temperature, its processing condition are: during 1240~1360 ℃ to 900 ℃, rate of temperature fall is 5~8 ℃/min; 900 ℃ to 500 ℃, rate of temperature fall is 3~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 4~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 8~10 ℃/min.
The present invention is in the process of preparation dichroite heat proof/refractory materials; Because lithium aluminium silicon series system glass is after bakingout process; Can form β-quartzy Solid solution and β-triphane Solid solution crystalline phase, make lithium silicon aluminum micro-crystal glass in big TR, have the property of low bulk even zero thermal expansion.Therefore, this material has extraordinary thermostability and high physical strength.Mix the lithium aluminium silicon series sytull as high temperature adhesives; When effectively having adjusted the powder stock sintering process and having prepared cordierite material; Liquid phase just can appear in problems such as the generation temperature of trichroite crystalline phase is high, firing range is narrow in the time of 1200 ℃, make total system separate out and burn till under the condition of temperature being lower than the trichroite crystalline phase; At this moment, a considerable amount of liquid phases appear in the system.When forming β-quartzy Solid solution and β-triphane Solid solution crystalline phase, because the existence of liquid phase makes the trichroite crystalline phase also can separate out.In 1240 ℃~1360 ℃ TR, burn till, can both obtain the dichroite heat proof/refractory materials of excellent property.
Below in conjunction with embodiment the present invention is described further, but does not limit the present invention.
Realize that the scheme that lithium aluminium silicon series system sytull combines trichroite to prepare the high-temperature heat-resistance material is:
Instance one:
The one, prepares burden according to the prescription that table 1 provides, and prepare lithium aluminium silicon series system glass with scorification, and shrend becomes glass powder.
The 2nd, trichroite chemical formulation is 2MgO2Al 2O 35SiO 2, theory consists of: MgO-13.78%, Al 2O 3-34.86%, SiO 2-51.36%.According to this metering, and be that raw material carries out charge calculation with talcum powder, aluminum oxide powder, kaolin.Each batching is a benchmark with the quality of 100 kilograms of oxide compounds, and charger sheet is seen table 3.
Be calculated as by charger sheet: talcum powder is 43.21 kilograms, and aluminum oxide powder is 14.79 kilograms, and kaolin is 51.35 kilograms, is 109.35 kilograms altogether.
The 3rd. on this basis, with 20% of each batching total mass, promptly 21.87 kilograms, mix lithium aluminium silicon series system glass powder, mix 1.5% Z 150PH (1.64 kilograms) and 42% water (45.93 public affairs) simultaneously.Putting into ball mill grinds, mixes.Milling time is 10~16 hours.Emit slip, and make it pass through 300 mesh sieves, screen over-size is 2~5%.
The 4th. utilize spraying drying with mud oven dry, granulation, and collect.And require to carry out moulding according to shape of products, moulding can be tabular, strip, bulk.Utilize the roller bed type drying kiln that base substrate is carried out drying after the moulding, dry body strength need reach more than the 3.8Mpa.
The 5th. following technology is adopted in burning till of shaping base substrate: from room temperature to 500 ℃, temperature rise rate≤1 ℃/min; 500 ℃ to 1100 ℃, temperature rise rate is 3 ℃/min, and by 1100 ℃ to 1200 ℃, temperature rise rate is 1 ℃/min; During 1200 ℃ of extremely final firing temperatures, 1.5 ℃/min of temperature rise rate ≈; Soaking time under the final calcining temperature is 2 to 5 hours; The type of cooling is: final firing temperature to 900 ℃, and rate of temperature fall is 5~8 ℃/min; 900 ℃ to 500 ℃, rate of temperature fall is 3~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 4~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 8~10 ℃/min.
The 6th. through X-ray diffraction analysis, the main crystalline phase that lithium aluminium silicon series system sytull combines trichroite to prepare in the high-temperature heat-resistance material is: a, trichroite, b, β-quartzy Solid solution, c, magnesium-aluminium spinel d, β-triphane Solid solution crystalline phase (Li xAl xSi 3-xO 6).Two main crystalline phases that comprised trichroite crystalline phase and lithium aluminium silicon series system sytull in this material.
The 7th. the performances such as expansion, thermal shock resistance through the lithium aluminium silicon series that burns till system sytull combines trichroite to prepare the high-temperature heat-resistance material are seen table 2.
Instance two:
The one, prepares burden according to the prescription that table 1 provides, and prepare lithium aluminium silicon series system glass with scorification, and shrend becomes glass powder.
The 2nd, trichroite chemical formulation is 2MgO2Al 2O 35SiO 2, design team becomes: MgO-15%, Al 2O 3-35%, SiO 2-50%.According to this metering, and be that raw material carries out charge calculation with magnesiumcarbonate, aluminum oxide powder, silica sand, the purity of raw material all is 98%.Each batching is a benchmark with the quality of 100 kilograms of oxide compounds, and be calculated as by charger sheet shown in the table 3: magnesiumcarbonate is 32.02 kilograms, and aluminum oxide powder is 35.71 kilograms, and silica sand is 51.02 kilograms, is 118.75 kilograms altogether.
The 3rd. on this basis,, promptly 17.81 kilograms, mix lithium aluminium silicon series system glass powder, mix 2.5% simultaneously with 15% of each batching total mass) Ucar 35 (2.97 kilograms and 40% water (47.5 kilograms).Putting into ball mill grinds, mixes.Milling time is 10~16 hours.Emit slip, and make it pass through 300 mesh sieves, screen over-size is 2~5%.
The 4th. utilize spraying drying with mud oven dry, granulation, and collect.And require to carry out moulding according to shape of products, moulding can be tabular, strip, bulk.Utilize the roller bed type drying kiln that base substrate is carried out drying after the moulding, dry body strength need reach more than the 3.8Mpa.
The 5th. following technology is adopted in burning till of shaping base substrate: from room temperature to 500 ℃, temperature rise rate≤1 ℃/min; 500 ℃ to 1100 ℃, temperature rise rate is 3 ℃/min, and by 1100 ℃ to 1200 ℃, temperature rise rate is 1 ℃/min; During 1200 ℃ of extremely final firing temperatures, 1.5 ℃/min of temperature rise rate ≈; Soaking time under the final calcining temperature is 2 to 5 hours; The type of cooling is: final firing temperature to 900 ℃, and rate of temperature fall is 5~8 ℃/min; 900 ℃ to 500 ℃, rate of temperature fall is 3~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 4~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 8~10 ℃/min.
The 6th. through X-ray diffraction analysis, the main crystalline phase that lithium aluminium silicon series system sytull combines trichroite to prepare in the high-temperature heat-resistance material is: a. trichroite, b. β-quartzy Solid solution, c. magnesium-aluminium spinel, d. β-triphane Solid solution crystalline phase (Li xAl xSi 3-xO 6).Two main crystalline phases that comprised trichroite crystalline phase and lithium aluminium silicon series system sytull in this material.
The lithium aluminium silicon series system sytull that the present invention adopts is meant with Li 2O-Al 2O 3-SiO 2System glass is the glass system on basis, under certain heat-treat condition, makes wherein a kind of microcrystal glass material of separating out, forming β-quartzy Solid solution, β-triphane Solid solution crystalline phase.The salient features of this material is low bulk (even zero thermal expansion or negative expansion can occur), and is high temperature resistant, heat shock resistance.During the lithium aluminium silicon series system sytull that this patent designed is formed, SiO 2With Al 2O 3Content very high, guaranteed the thermostability that it had.
Subordinate list
The chemical constitution (quality %) of table 1 lithium aluminosilicate glass
Composition SiO 2 Al 2O 3 B 2O 3 MgO TiO 2 ZrO 2 Li 2O ZnO Na 2O Sb 2O 3
Wt% 64.00 23.00 0.50 2.50 2.00 2.00 4.00 1.00 0.5 0.5
The performance index of the dichroite heat proof/refractory materials of table 2 preparation
Sequence number Performance Unit Indication range
1 Thermal expansivity 1/K 0.8—3.4×10 -6
2 Thermal shock performance 1100—1200
3 Folding strength MPa 32.26—68.42
4 Void content 26.63—41.48
Table 3 charger sheet
Oxide compound MgO (kilogram) Al 2O 3(kilogram) SiO 2(kilogram) H 2O (kilogram) Consumption (kilogram)
Talcum powder 13.78 - 27.39 2.04 43.21
Kaolin 20.37 23.79 7.19 51.35
Aluminum oxide powder - 14.49 - 14.79
Add up to 109.35

Claims (4)

1. the preparation method of a dichroite heat proof/refractory materials is characterized in that the lithium aluminium silicon series glass powder of uniting is incorporated in the preparation dichroite heat proof/refractory materials raw material, and with they together ball mill mixing, process, specifically be the method that adopts following steps:
(1) batching: by weight, take by weighing Al earlier 2O 330~50%, MgO 8~20%, SiO 240~60%, mix lithium aluminium silicon series system glass powder by 5~25% of the raw material total mass that takes by weighing at every turn again, get mixture,
By weight percentage, consisting of of said lithium aluminium silicon series system glass powder: SiO 264%, Al 2O 323.00%, B 2O 30.50%, MgO 2.50%, TiO 22.00%, ZrO 22.00%, Li 2O 4.00%, and ZnO 1.00%, Na 2O 0.5%, Sb 2O 30.5%;
(2) ball mill mixing: mixture is put into ball mill, and again by the mixture total mass, the water of adding 35~50%, 1~3% organic additive mixed, grind 10~16 hours, filtered through 300 mesh sieves then, got slip;
(3) prepare base substrate: after slip is carried out spraying drying and granulation, get base substrate through compression moulding, the shape of base substrate is sheet, strip or bulk;
(4) blank sintering:
Room temperature progressively rises to 1240~1360 ℃ base substrate carried out sintering, and is incubated 2~5 hours, and the process that is progressively risen to 1200 ℃ by room temperature is: from room temperature to 500 ℃, temperature rise rate is≤1 ℃/min; 500 ℃ to 1100 ℃, temperature rise rate is 3 ℃/min, and by 1100 ℃ to 1200 ℃, temperature rise rate is 1 ℃/min,
Progressively be cooled to room temperature again, in the process that progressively is cooled to room temperature, its processing condition are: during 1240~1360 ℃ to 900 ℃, rate of temperature fall is 5~8 ℃/min; 900 ℃ to 500 ℃, rate of temperature fall is 3~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 4~5 ℃/min; 500 ℃ to 200 ℃, rate of temperature fall is 8~10 ℃/min;
Through above-mentioned steps, obtain described dichroite heat proof/refractory materials.
2. the preparation method of dichroite heat proof/refractory materials according to claim 1, it is characterized in that: organic additive is Z 150PH or USP Kosher.
3. the preparation method of dichroite heat proof/refractory materials according to claim 1 is characterized in that: when compression moulding, it is half-dried molded to adopt 1800~2200 tons press to carry out earlier, utilizes the roller bed type dry kiln that compacted products is carried out drying then.
4. the preparation method of dichroite heat proof/refractory materials according to claim 1 is characterized in that: the main crystalline phase in the said dichroite heat proof/refractory materials be the trichroite crystalline phase with lithium aluminium silicon series system sytull mutually.
CN2008101972077A 2008-10-09 2008-10-09 Method for preparing dichroite heat proof/refractory materials Expired - Fee Related CN101381240B (en)

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CN102603277B (en) * 2011-01-19 2014-09-03 比亚迪股份有限公司 Preparation method for cordierite
CN102408181B (en) * 2011-08-30 2013-11-13 河北省沙河玻璃技术研究院 Preparation method of borosilicate float glass batch
CN102924068B (en) * 2012-11-15 2014-05-07 景德镇陶瓷学院 Wall-flow honeycomb ceramic filter for high-temperature exhaust gas purification, and preparation method thereof
CN104310417B (en) * 2014-10-08 2016-06-29 武汉科技大学 A kind of containing zirconium cordierite composite diphase material and preparation method thereof
CN105271763B (en) * 2015-11-20 2017-11-24 中国地质大学(武汉) It is a kind of using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material and preparation method thereof
NL2019716B1 (en) * 2016-10-13 2018-08-14 Schott Ag Cordierite glass-ceramic, production and use thereof
CN109851337A (en) * 2019-01-08 2019-06-07 广东山摩新材料科技有限公司 A kind of high temperature dichroite-mullite refractory slab and preparation method thereof
CN110054484A (en) * 2019-05-07 2019-07-26 安徽普瑞普勒传热技术有限公司 A kind of heat-exchange ceramic and preparation method thereof

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