CN105481382A - Preparation method of cordierite fireproof material - Google Patents

Preparation method of cordierite fireproof material Download PDF

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Publication number
CN105481382A
CN105481382A CN201410478092.4A CN201410478092A CN105481382A CN 105481382 A CN105481382 A CN 105481382A CN 201410478092 A CN201410478092 A CN 201410478092A CN 105481382 A CN105481382 A CN 105481382A
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cordierite
temperature
rate
refractory
room temperature
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CN201410478092.4A
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韩君昌
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Qingdao Baijiancheng Environmental Protection Technology Co Ltd
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Qingdao Baijiancheng Environmental Protection Technology Co Ltd
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Abstract

The invention provides a preparation method of a cordierite fireproof material. The preparation method comprises the following steps of mixing lithium-aluminum-silicon system graphite powder with raw materials for preparing the cordierite fireproof material, and ball-milling the mixture of the lithium-aluminum-silicon system graphite powder and the raw materials, and performing mixing and processing. The cordierite fireproof material contains a cordierite crystalline phase and a lithium-aluminum-silicon system microcrystalline glass crystalline phase. The fireproof material prepared by the method not only is good in quality and high in properties, but also is reduced in energy consumption, the average firing temperature of the fireproof material is 100-120 DEG C lower than that of a conventional method, the range of the firing temperature is extended by 80-100 DEG C, and besides, the technology is simple, practical and reliable.

Description

A kind of preparation method of cordierite refractory material
Technical field
The present invention relates to technical field of refractory materials, particularly relate to a kind of preparation method of cordierite refractory material.
Background technology
Be the heat-resisting of principal crystalline phase or refractory materials with trichroite, there is very excellent performance.Because light weight, thermal conductivity are low, use temperature is relatively high and be used directly on flame front, thus reaches energy-efficient effect.What also have is used on the higher heat exchanger of cold and hot exchange frequency, as durable heat pot, and the heat resisting porcelain on gas furnace, honeycomb kitchen range etc.
The development of cordierite material has the history of more than 100 year.1899, the artificial lens " Cordierite " that first L.Morozewic obtains, i.e. trichroite.1918, Rankin and Merwin was at research MgO-A1 20 3-Si0 2in the process of three-part system, synthesize α-type ternary compound, and thought that α-type is identical with the trichroite that L.Morozewicz synthesizes, also identical with natural trichroite.The result of study of nineteen fifty-five Miyashiroetal shows that α-cordierite is hexagonal system, and β mono-trichroite may be rhombic system, both different from natural trichroite.Mineralogically, the method for employing optics and XRD determines the difference between α-type and β-type trichroite, and chemical formula Mg2A14Si5018 has two polymorphous modification series: one is hexagonal system, and another the present is rhombic system.Afterwards, the performance of a large amount of researchist to trichroite conducts in-depth research, and the thermostability that especially trichroite is good and the low coefficient of expansion receive much attention.In actual production, late 1980s, produced the low bulk cordierite articles that Performance comparision is excellent, the quality of cordierite articles improves with benefit.The cordierite-quality honeycombed ceramics that such as Corning Incorporated produces, its thermal expansivity (Rt ~ l00 DEG C) is 1.0 ~ 1.2xl0 -6/ DEG C, heat-shock resistance reaches 700 DEG C.
Comprehensive both at home and abroad about the research and preparation of cordierite material can find, prepare the main raw material of cordierite material, proportioning is Si0 2-50.15%, A1 20 3-34.04%, Mg0-13.46%, under the condition of 1350 DEG C, burn till more than 3 hours, just can prepare the coefficient of expansion is 1.6-2.4xl0 -6the trichroite of/DEG C (22 ~ 800 DEG C).
Cordierite ceramic take cordierite crystal as principal crystalline phase.Cordierite ceramic thermal refractory material adopts two kinds of method manufactures usually, and one is melten glass crystallization process, and another kind is powder stock sintering process.
Melten glass crystallization process is that the admixtion mixed is formed glass through high-temperature fusion, after shaping, then heat-treat crystallize out and makes cordierite ceramic.This method requires that glass smelting is even, bubble-free, and melt temperature also should be high, reaches more than 1600 DEG C.Powder stock sintering rule is founded at relatively low temperature, and wear into fine powder after shrend, carry out sintering and obtaining cordierite ceramic after shaping, this method is burnt till humidity and can be controlled in less than 1450 DEG C and carry out.
The cordierite material of sintering synthesis is with talcum, kaolin or clay and aluminum oxide etc. for raw material, by three kinds of raw materials by suitable proportion mixed preparing, in sintering procedure, forms synthesis of dichroite.For being reduced in sintering procedure the thermal expansivity forming synthesis of dichroite, selected suitable raw material composition is very important, and the proportioning raw materials of usual synthesis of dichroite all draws according to trichroite phasor, and this compositing area is at Si0 2-A1 20 3with cordierite crystal phase composite point (2Mg0 in-Mg0 system phasor 2a1 20 35Si0 2) centered by narrow and small compositing range, have data to show, if its chemical constitution point is respectively near rich Mg0 side, rich A1 20 3some composition points of side, then cordierite ceramic will have lower thermal expansivity.Usually, the proportioning (by weight) of green stock mixture is: the A1 of 30%-50% 20 3,the Si0 of the Mg0 of 8%-20%, 40%-60% 2, and can certain adjustment be carried out.
Because natural trichroite quantity is few, poor performance.Make goods both have certain intensity, have again longer work-ing life, and towards the future development of energy-conservation, high-quality, high yield, generally must adopt the A1 of high pure and ultra-fine 20 3, Mg0 and Si0 2powder synthesizes high-purity trichroite, and firing temperature is up to 1350 ~ 1440 DEG C.Raw materials cost is high, energy consumption is large, so bringing a high price of high-purity trichroite synthesis material, thus can not apply 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 formed in crystal is low, the diffusion of unfavorable particle, make solid-phase reaction velocity slow like this, sintered density is poor, have impact on intensity and the work-ing life of cordierite material.The existence of some impurity in raw material, not only can improve the firing range of trichroite, and substantially increases the work-ing life of cordierite material.
The process characteristic of cordierite goods is generation temperature high (about 1400 DEG C) of trichroite, and fusing point low (about 1460 DEG C are decomposed into mullite and contain magnesium liquid phase), cause the firing range of cordierite goods narrow.Do not have the trichroite of significant amounts to generate at a lower temperature, goods can not sinter; Improve calcining temperature, a large amount of slopes glass can be caused to generate mutually, reduce the thermostability of cordierite goods.
The temperature range of burning till trichroite is narrow, thus in fact, often adds as Na in production process 20, K 20, Ca0, Ba0, Fe 20 3and Ti0 2etc. a small amount of impurity, they can reduce temperature of fusion can expand melting range again.Ca0, Na 20, K 20, Fe 20 3deng all can the formation of participation cordierite crystal structure in various degree, Ca0, Fe 20 3mg can be replaced 2+form substitutional solid solution.Because Ca2+ ionic radius is greater than Mg 2+, after entering trichroite, cause character to distort, form stress room, thus can synthesis temperature be reduced, sintering range is broadened.Appropriate Fe 20 3can firing range be widened, but work as Fe 20 3during more than 0.65%, then thermal expansivity can sharply rise.Ti0 2, Ba0, Zr0 2deng all can reduction thermal expansivity in various degree.The introducing of these admixtures can improve and promote can improve again the thermal shock resistance of material by the sintering of trichroite.
Exist in the burning till of cordierite refractory material at present: 1. firing temperature is up to 1360 ~ 1440 DEG C; The temperature range 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 problem existing for cordierite refractory material for above powder stock sintering process, thering is provided a kind of and novel be suitable for industrialized preparing process, to preparing, there is good quality, performance and the cordierite refractory material in work-ing life.
The technical scheme that the present invention solves the employing of its technical problem is: a kind of preparation method of cordierite refractory material, being incorporated into by lithia-alumina-silica system Graphite Powder 99 prepares in cordierite refractory material feedstock, and with they together ball milling mix, process, specifically adopt the method for following steps:
L () is prepared burden: by weight, first take A 120 325 ~ 45%, Mg05 ~ 15%, Si0 235 ~ 55%, then mix lithia-alumina-silica system Graphite Powder 99 by 5 ~ 15% of the raw material total mass taken at every turn, obtain mixture;
(2) ball milling mixing: mixture is put into ball mill, then by mixture total mass, add the water of 35 ~ 45%, 1 ~ 3% polyvinyl alcohol carry out mixing, grinding 12 ~ 18 hours, then through 300 mesh screen, obtain slip;
(3) prepare base substrate: after carrying out spraying dry and granulation to slip, repressed shaping base substrate, the shape of base substrate can be sheet, strip or bulk;
(4) blank sintering: progressively rise to 1250 ~ 1350 DEG C by room temperature and sinter base substrate, and be incubated 3 ~ 5 hours, be more progressively cooled to room temperature, obtains described cordierite refractory material.
It is characterized in that the process progressively rising to 1200 DEG C by room temperature is: from room temperature to 500 DEG C, temperature rise rate is≤1 DEG C/min; 500 DEG C to 1100 DEG C, temperature rise rate is 3 DEG C/min, and by 1100 DEG C to 1200 DEG C, temperature rise rate is 1 DEG C/min.
It is characterized in that progressively being cooled in the process of room temperature, its processing condition are: 1250 ~ 1350 DEG C to 900 DEG C periods, rate of temperature fall is 5 ~ 8 DEG C/min; 900 DEG C to 500 DEG C, rate of temperature fall is 3 ~ 5 DEG C/min; 500 DEG C to 200 DEG C, rate of temperature fall is 4 ~ 5 DEG C/min:500 DEG C to 200 DEG C, rate of temperature fall is 8 ~ 10 DEG C/min.
When compression moulding, first adopt the press of 1800 ~ 2200 tons to carry out half dry-pressing formed, then utilize roller bed type dry kiln to carry out drying to compacted products.
Principal crystalline phase in described cordierite refractory material is cordierite crystalline phase and lithia-alumina-silica system devitrified glass crystalline phase.
Compared with the present invention prepares cordierite material method with existing powder stock sintering process, its advantage is mainly: by mixing lithia-alumina-silica system Graphite Powder 99, fully utilize the characteristic and advantage of this powder and this bi-material of trichroite, at relatively low with wide in range temperature, prepare and there is good quality and performance and the refractory materials compared with the long life, in this material, contain two principal crystalline phase of cordierite crystalline phase and lithia-alumina-silica system devitrified glass.Utilize the refractory materials that our legal system is each, its firing temperature on average reduces by 100 ~ 120 DEG C than traditional method, and firing range expands 80 ~ 100 DEG C, and therefore energy consumption decreases.The incorporation of lithia-alumina-silica system Graphite Powder 99 can control in 5% ~ 25% of each batching total mass.
Present method technique is simple, practical and reliable, is suitable for suitability for industrialized production.
Embodiment
Cordierite refractory MATERIALS METHODS of preparing provided by the invention is: be incorporated into by lithia-alumina-silica system Graphite Powder 99 and prepare in cordierite refractory material feedstock, and with they together ball milling mix, process.
Specifically adopt the method for following steps:
L () is prepared burden: by weight, first take A 120 337%, Mg07%, Si0 248%, then mix lithia-alumina-silica system Graphite Powder 99 by 8% of the raw material total mass taken at every turn, obtain mixture;
(2) ball milling mixing: mixture is put into ball mill, then by mixture total mass, add the water of 36%, 2% polyvinyl alcohol carry out mixing, grinding 14 hours, then through 300 mesh screen, obtain slip;
(3) prepare base substrate: after carrying out spraying dry and granulation to slip, repressed shaping base substrate, the shape of base substrate can be sheet, strip or bulk;
(4) blank sintering: progressively rise to 1290 DEG C by room temperature and sinter base substrate, and be incubated 3 ~ 5 hours, be more progressively cooled to room temperature, obtains described cordierite refractory material.
The process progressively being risen to 1200 DEG C by room temperature is: from room temperature to 500 DEG C, and temperature rise rate is≤1 DEG C/min; 500 DEG C to 1100 DEG C, temperature rise rate is 3 DEG C/min, and by 1100 DEG C to 1200 DEG C, temperature rise rate is 1 DEG C/min.
Progressively be cooled in the process of room temperature, its processing condition are: 1250 ~ 1350 DEG C to 900 DEG C periods, rate of temperature fall is 5 ~ 8 DEG C/min; 900 DEG C to 500 DEG C, rate of temperature fall is 3 ~ 5 DEG C/min; 500 DEG C to 200 DEG C, rate of temperature fall is 4 ~ 5 DEG C/min:500 DEG C to 200 DEG C, rate of temperature fall is 8 ~ 10 DEG C/min.
When compression moulding, first adopt the press of 1800 ~ 2200 tons to carry out half dry-pressing formed, then utilize roller bed type dry kiln to carry out drying to compacted products.
Principal crystalline phase in described cordierite refractory material is cordierite crystalline phase and lithia-alumina-silica system devitrified glass crystalline phase.
The present invention is in the process preparing cordierite refractory material, because lithia-alumina-silica system glass is after Overheating Treatment, β-quartzy Solid solution and β mono-triphane Solid solution crystalline phase can be formed, make lithium silicon aluminum micro-crystal glass in large temperature range, have the low bulk even property of zero thermal expansion.Therefore, this material has extraordinary thermostability and high physical strength.Mix lithium aluminosilicate glass-ceramics as high temperature adhesives, effectively have adjusted powder stock sintering process when preparing cordierite material, the problems such as the generation temperature of cordierite crystalline phase is high, firing range is narrow, just liquid phase can be there is 1200 DEG C time, whole system is burnt till under the condition lower than cordierite crystalline phase Precipitation Temperature, now, there is a considerable amount of liquid phase in system.While formation β-quartzy Solid solution and β-triphane Solid solution crystalline phase, due to the existence of liquid phase, cordierite crystalline phase also can be separated out.Burn till in the temperature range of 1240 DEG C ~ 1360 DEG C, the cordierite refractory material of excellent property can both be obtained.

Claims (5)

1. a preparation method for cordierite refractory material, is characterized in that lithia-alumina-silica system Graphite Powder 99 to be incorporated into prepare in cordierite refractory material feedstock, and with they together ball milling mix, process, specifically adopt the method for following steps:
L () is prepared burden: by weight, first take A 120 325 ~ 45%, Mg05 ~ 15%, Si0 235 ~ 55%, then mix lithia-alumina-silica system Graphite Powder 99 by 5 ~ 15% of the raw material total mass taken at every turn, obtain mixture;
(2) ball milling mixing: mixture is put into ball mill, then by mixture total mass, add the water of 35 ~ 45%, 1 ~ 3% polyvinyl alcohol carry out mixing, grinding 12 ~ 18 hours, then through 300 mesh screen, obtain slip;
(3) prepare base substrate: after carrying out spraying dry and granulation to slip, repressed shaping base substrate, the shape of base substrate can be sheet, strip or bulk;
(4) blank sintering: progressively rise to 1250 ~ 1350 DEG C by room temperature and sinter base substrate, and be incubated 3 ~ 5 hours, be more progressively cooled to room temperature, obtains described cordierite refractory material.
2. the preparation method of cordierite refractory material according to claim 1, is characterized in that the process progressively rising to 1200 DEG C by room temperature is: from room temperature to 500 DEG C, temperature rise rate is≤1 DEG C/min; 500 DEG C to 1100 DEG C, temperature rise rate is 3 DEG C/min, and by 1100 DEG C to 1200 DEG C, temperature rise rate is 1 DEG C/min.
3. the preparation method of cordierite refractory material according to claim 1, it is characterized in that progressively being cooled in the process of room temperature, its processing condition are: 1250 ~ 1350 DEG C to 900 DEG C periods, rate of temperature fall is 5 ~ 8 DEG C/min; 900 DEG C to 500 DEG C, rate of temperature fall is 3 ~ 5 DEG C/min; 500 DEG C to 200 DEG C, rate of temperature fall is 4 ~ 5 DEG C/min:500 DEG C to 200 DEG C, rate of temperature fall is 8 ~ 10 DEG C/min.
4. the preparation method of cordierite refractory material according to claim 1, is characterized in that: when compression moulding, first adopts the press of 1800 ~ 2200 tons to carry out half dry-pressing formed, then utilizes roller bed type dry kiln to carry out drying to compacted products.
5. the preparation method of cordierite refractory material according to claim 1, is characterized in that: the principal crystalline phase in described cordierite refractory material is cordierite crystalline phase and lithia-alumina-silica system devitrified glass crystalline phase.
CN201410478092.4A 2014-09-19 2014-09-19 Preparation method of cordierite fireproof material Pending CN105481382A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106365669A (en) * 2016-08-31 2017-02-01 山东奥福环保科技股份有限公司 Cordierite honeycomb ceramic carrier using complete oxides as raw materials and preparation method thereof
CN107151148A (en) * 2017-05-11 2017-09-12 焦作诺尔曼炉业有限公司 A kind of cordierite thermal insulation fire-resistant ball and preparation method thereof
CN107935397A (en) * 2016-10-13 2018-04-20 肖特股份有限公司 Cordierite glass-ceramic, its production method and purposes

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106365669A (en) * 2016-08-31 2017-02-01 山东奥福环保科技股份有限公司 Cordierite honeycomb ceramic carrier using complete oxides as raw materials and preparation method thereof
CN106365669B (en) * 2016-08-31 2019-05-21 山东奥福环保科技股份有限公司 It is a kind of using total oxygen compound as cordierite honeycomb ceramic carrier of raw material and preparation method thereof
CN107935397A (en) * 2016-10-13 2018-04-20 肖特股份有限公司 Cordierite glass-ceramic, its production method and purposes
CN107151148A (en) * 2017-05-11 2017-09-12 焦作诺尔曼炉业有限公司 A kind of cordierite thermal insulation fire-resistant ball and preparation method thereof

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Application publication date: 20160413