CN105294081A - Preparation method of Al5O6N-combined corundum composite refractory material - Google Patents

Preparation method of Al5O6N-combined corundum composite refractory material Download PDF

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Publication number
CN105294081A
CN105294081A CN201510833909.XA CN201510833909A CN105294081A CN 105294081 A CN105294081 A CN 105294081A CN 201510833909 A CN201510833909 A CN 201510833909A CN 105294081 A CN105294081 A CN 105294081A
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China
Prior art keywords
corundum
preparation
al5o6n
raw material
refractory material
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CN201510833909.XA
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Chinese (zh)
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李勇
秦海霞
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Pending legal-status Critical Current

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Abstract

The invention belongs to the field of an inorganic nonmetallic material, and relates to a preparation method of a Al5O6N-combined corundum refractory material, which is used for preparing a refractory material for an iron making blast furnace, a steel making steel ladle, a secondary refining furnace, a kiln mouth and a transition belt of a cement rotary kiln, a kiln product, and the like. Tabular corundum, white corundum, and activated alumina micro-powder are adopted as raw materials; a phenolic resin is added and is taken as a binding agent; the obtained product is subjected to pressing, nitridation, and sintering; and the Al5O6N-combined corundum composite refractory material is prepared through a simple process of reacting carbon residue after resin sintering with activated alumina micro-powder under the atmosphere of nitrogen. The preparation method is simple in process, free of complex device, and low in cost, and causes small environmental pollution during a production process. The prepared refractory material is not prone to cause recarburization of liquid steel, and is easy for industrial promotion.

Description

A kind of Al 5o 6the preparation method of the combining corundum based composite refractory of N
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to Al 5o 6the preparation method of N combining corundum based refractory materials, for the preparation of iron-smelting blast furnace, steel-making ladle, external refining stove and cement kiln refractory.
AlON is a kind of Al 2o 3the sosoloid of-AlN two component system, owing to having the advantage of non-compound and oxide compound concurrently, there is the excellent properties such as good high thermal resistance and the rotten candle of oxidation-resistance, exceptional hardness, high melting-point, high thermoconductivity and chemically-resistant, high-temperature structural ceramics, high-performance refractory material and high-performance window pyrometer gate material, can be used as the high-temperature component of grinding medium, metal-cutting machine tool, binder for fire-resistant materials, heat engine or other thermal hardwares, can be used as again sealing-ring, bearing, valve body etc., because it has good light transmission, also crystalline ceramics can be prepared.Current research mainly concentrates on AlON crystalline ceramics.
People find in refractory system applied research AlON, AlON composite alumina, match grand etc., and its advantage is more outstanding under the high temperature conditions.Because they have high temperature resistant, anti-oxidant, that intensity is high, hardness is large and anti-erosion etc. is excellent performance, so can improve refractory materials long service life.There is vast potential for future development in fields such as ferrous metallurgy, building materials, chemical industry, machinery and kiln furniture materials, can be used as iron-smelting blast furnace shaft bottom, furnace bosh, cupola well, ceramic cup ceramic blanket etc., also can be used as blast furnace cleek material; Steel-making ladle and external refining refractory materials.Rotary cement kiln eye etc.
But in AlON system, about Al 5o 6the report of N is less.There is investigator with AlN, Al 2o 3, CeO 2, Tb 4o 7as raw material, in nitrogen atmosphere, 1700 DEG C are heated 4 hours, obtain Al 5o 6n:Ce 3+, Tb 3+material, studies its luminescent properties as fluorescent agent; Preparation method more at present adopts TNT explosive and metal A l powder as raw material, collects recrement filtration and dissolves, after calcining, obtain Al after igniting 5o 6n powder, the method needs to adopt explosive initiation, comparatively dangerous, and metallic aluminium powder is not easily taken care of, and cost higher being therefore difficult to realizes industrialized mass production.
About Al 5o 6n is more rare at the report of Application in Refractory, has investigator with α-Al 2o 3micro mist, metallic aluminium powder, simple substance silica flour, crystalline flake graphite, and resol is as bonding agent, AlN powder has prepared Al as additive 5o 6the Al that N combines 2o 3-C refractory materials, can improve about 30MPa by cold crushing strength, and residual strength after thermal shock is improved 18MPa.This research shows Al 5o 6n can play REINFORCED Al 2o 3the effect of-C refractory materials.But the process employs metallic aluminium powder and simple substance silica flour two kinds raw material costly, and preserve improper explosive, and crystalline flake graphite in addition, the in use too much carbon of refractory materials may be caused to cause molten steel recarburization.
Summary of the invention:
Al has been prepared with AlN powder as additive in the middle of prior art 5o 6the Al that N combines 2o 3-C refractory materials, the defect that cost is high, carbon left is high, provides a kind of available Al 5o 6the preparation method of the combining corundum based composite refractory of N.Compared with other preparation methods, feed composition is simple, cheap and easy to get; Simple for process, without the need to applying pressure; Adopt the carbon residue after heat-reactive phenolic resin high-temperature ammonolysis as carbon source, low-carbon environment-friendly, economizes on resources; Do not add the raw material of the costlinesses such as rare metal, greatly reduce industrial cost.
A preparation method for the combining corundum based composite refractory of Al5O6N, is characterized in that: described material adopts plate diamond spar, white fused alumina, Reactive alumina as raw material, adds resol as bonding agent, repressedly shapingly nitridation sinteredly to form afterwards; After shaping, wherein plate diamond spar forms refractory materials skeleton as macrobead, corundum as in particles filled, alumina powder is as matrix; After Nitride firing, Reactive alumina forms Al through reaction 5o 6n, as in conjunction with phase, strengthens corundum material.
Al in raw material 2o 3micro mist is fabricated in situ under nitrogen atmosphere, resin high temperature carbon residue condition, is present in mutually in matrix as combination.
Massfraction 40-60% got by raw material is plate diamond spar macrobead, and 15-35% is particle in corundum, 5-25% Reactive alumina, adds the 3-5% resol of raw material in addition, carries out mixing, compression moulding under 15-40MPa after being mixed by raw material; Sample after compression moulding being put into sintering oven, leading to purity for being not less than 99.99% nitrogen, naturally cooling after carrying out nitrogenize 8-24h at 1600-2000 DEG C.
The performance of material prepared by the present invention is void content 10-19%, volume density 3.10-3.25g/cm 3, cold crushing strength 100-480MPa is the brick that a kind of intensity is larger, suitable to blast furnace, ladle and external refining and cement kiln brick.
Basic conception of the present invention is with plate diamond spar, white fused alumina, and Reactive alumina is as raw material, and heat-reactive phenolic resin, as bonding agent, reacts under high temperature nitrogen atmosphere, fabricated in situ Al 5o 6n, strengthens corundum refractory mutually as combination.The present invention breaches industrial technology and prepares Al 5o 6n must add the limitation of elemental metals and additive, with Al 2o 3for raw material, prepare Al 5o 6n combined corundum composite refractory.
With corundum in granules material and alumina powder for raw material, thermoset phenolic resin, as bonding agent, utilizes resin carbon residue after sintering, reacts in nitrogen atmosphere with Reactive alumina, preparation Al 5o 6the corundum refractory that N combines.Preparation method that the present invention adopts does not add elemental metals, with low cost, and safety preserved by raw material, there is not explosion hazard; Do not adopt graphite, only utilize the carbon residue after phenolic resin binder high temperature sintering, low-carbon environment-friendly; Do not adopt the thuliums such as Ce, Tb, economize on resources, greatly reduce costs; Do not adopt AlN additive; Only employing 1600-2000 DEG C is nitridation sintered, does not apply pressure, technique simple possible.The present invention adopts raw material cheap and easy to get, and the simple technique of environmental protection prepares the Al of superior performance 5o 6n composite material combined with corundum, industrialization promotion is convenient in pole.
Specific implementation method:
Getting 40-60% by massfraction is plate diamond spar macrobead, and 15-35% is particle in corundum, 5-25% Reactive alumina, adds 3-5% resol in addition as bonding agent, carries out mixing after being mixed by raw material, and compression moulding under 15-40MPa.Sample after compression moulding is put into sintering oven, and logical purity is 0.9999 nitrogen, and naturally cooling after carrying out nitrogenize 8-24h at 1600-2000 DEG C, prepares Al 5o 6the combining corundum based composite refractory of N.
Example 1
Get the plate diamond spar macrobead of 60% by massfraction, particle in 25% corundum, 15% Reactive alumina, add 5% resol in addition as bonding agent, carry out mixing after raw material is mixed, and compression moulding under 20MPa.Sample after compression moulding is put into sintering oven, and logical purity is 0.9999 nitrogen, and naturally cooling after carrying out nitrogenize 8-24h at 1700 DEG C, prepares Al 5o 6the combining corundum based composite refractory of N.
Example 2
Get the plate diamond spar macrobead of 60% by massfraction, particle in 25% corundum, 15% Reactive alumina, add 5% resol in addition as bonding agent, carry out mixing after raw material is mixed, and compression moulding under 20MPa.Sample after compression moulding is put into sintering oven, and logical purity is 0.9999 nitrogen, and naturally cooling after carrying out nitrogenize 8-24h at 1800 DEG C, prepares Al 5o 6the combining corundum based composite refractory of N.
Example 3:
Get the plate diamond spar macrobead of 40% by massfraction, particle in 35% corundum, 25% Reactive alumina, add 3% resol in addition as bonding agent, carry out mixing after raw material is mixed, and compression moulding under 15MPa.Sample after compression moulding is put into sintering oven, and logical purity is 0.9999 nitrogen, and naturally cooling after carrying out nitrogenize 8-24h at 1800 DEG C, prepares Al 5o 6the combining corundum based composite refractory of N.

Claims (4)

1. the preparation method of the combining corundum based composite refractory of Al5O6N, it is characterized in that: described material adopts plate diamond spar, white fused alumina, Reactive alumina as raw material, add resol as bonding agent, repressedly shapingly nitridation sinteredly to form afterwards; After shaping, wherein plate diamond spar forms refractory materials skeleton as macrobead, corundum as in particles filled, alumina powder is as matrix; After Nitride firing, Reactive alumina forms Al through reaction 5o 6n, as in conjunction with phase, strengthens corundum material.
2. the preparation method of the combining corundum based composite refractory of Al5O6N according to claim 1, is characterized in that: the Al in raw material 2o 3micro mist is fabricated in situ under nitrogen atmosphere, resin high temperature carbon residue condition, is present in mutually in matrix as combination.
3. the preparation method of the combining corundum based composite refractory of Al5O6N according to claim 1, it is characterized in that: massfraction 40-60% got by raw material is plate diamond spar macrobead, 15-35% is particle in corundum, 5-25% Reactive alumina, add the 3-5% resol of raw material in addition, carry out mixing after raw material is mixed, compression moulding under 15-40MPa; Sample after compression moulding being put into sintering oven, leading to purity for being not less than 99.99% nitrogen, naturally cooling after carrying out nitrogenize 8-24h at 1600-2000 DEG C.
4. the preparation method of the combining corundum based composite refractory of Al5O6N according to claim 1, is characterized in that: the performance of prepared material is void content 10-19%, volume density 3.10-3.25g/cm 3, cold crushing strength 100-480MPa.
CN201510833909.XA 2015-11-25 2015-11-25 Preparation method of Al5O6N-combined corundum composite refractory material Pending CN105294081A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106588024A (en) * 2017-01-05 2017-04-26 北京科技大学 Preparation method for Al<7>O<3>N<5> combined corundum composite refractory material
CN110023268A (en) * 2016-12-28 2019-07-16 黑崎播磨株式会社 The manufacturing method of the State of Blast Furnace bed portions and State of Blast Furnace bed portions brick of State of Blast Furnace bed portions brick and use State of Blast Furnace bed portions brick
CN112479688A (en) * 2020-11-27 2021-03-12 云南濮耐昆钢高温材料有限公司 Prevent blockking up gas pocket high dispersion air brick for anode furnace copper smelting
CN115477544A (en) * 2022-10-31 2022-12-16 安徽瑞泰新材料科技有限公司 Corrosion-resistant refractory material and preparation method thereof

Citations (1)

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CN103214256A (en) * 2013-05-10 2013-07-24 北京科技大学 Al23O27N5-combined corundum composite slide plate and preparation method thereof

Patent Citations (1)

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CN103214256A (en) * 2013-05-10 2013-07-24 北京科技大学 Al23O27N5-combined corundum composite slide plate and preparation method thereof

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Title
李传静等: "氮气气氛下制备的Al-Si3N4-Al2O3复合材料的显微结构及性能", 《硅酸盐学报》 *
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110023268A (en) * 2016-12-28 2019-07-16 黑崎播磨株式会社 The manufacturing method of the State of Blast Furnace bed portions and State of Blast Furnace bed portions brick of State of Blast Furnace bed portions brick and use State of Blast Furnace bed portions brick
EP3564201A4 (en) * 2016-12-28 2020-08-19 Krosakiharima Corporation Brick for blast furnace hearths and blast furnace hearth using same, and method for producing brick for blast furnace hearths
CN106588024A (en) * 2017-01-05 2017-04-26 北京科技大学 Preparation method for Al<7>O<3>N<5> combined corundum composite refractory material
CN112479688A (en) * 2020-11-27 2021-03-12 云南濮耐昆钢高温材料有限公司 Prevent blockking up gas pocket high dispersion air brick for anode furnace copper smelting
CN115477544A (en) * 2022-10-31 2022-12-16 安徽瑞泰新材料科技有限公司 Corrosion-resistant refractory material and preparation method thereof

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Application publication date: 20160203