CN106316426B - A kind of Resisting fractre refractory material and its preparation process - Google Patents
A kind of Resisting fractre refractory material and its preparation process Download PDFInfo
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Abstract
The invention discloses a kind of Resisting fractre refractory material and its preparation process, refractory material is made by raw materials such as aluminium oxide-silicon oxide mixed powder, calcium oxide, magnesia, manganese oxide, titanium oxide, niobium pentaoxide and toughened fibers；Its preparation step is that ball milling mixes raw material stoving after ball milling mixing in dehydrated alcohol after mixing above-mentioned raw materials, dry-pressing formed later, and refractory material green compact are made；Then it is sintered, cooled to room temperature after the completion of sintering, Resisting fractre refractory material is made.Refractory material mechanical tenacity with higher produced by the present invention and good break resistance, while there is excellent thermal shock resistance；Refractory material preparation method is simple, is easy to produce into the heart on existing.
Description
Technical field
The present invention relates to technical field of refractory materials, more particularly, to a kind of Resisting fractre refractory material and its preparation process.
Background technique
In traditional sense, refractory material refers to that refractoriness is not less than 1580 DEG C of inorganic non-metallic material, it is for height
The basic material of temperature technique service is used as structural material and industrial high temperature container and the portion of the Thermal Equipments such as high temperature kiln
The material of part, and it is able to bear corresponding physicochemical change and mechanism.
Most of refractory material is with natural crystal (such as fire clay, silica, magnesite, dolomite) for raw material manufacture
, using certain raw materials of industry and artificial-synthetic material (such as commercial alumina, silicon carbide, mullite synthesizing, synthetic spinel
Deng) also increasing, therefore, there are many type of refractory material.Refractory material can be divided into according to mineral composition aoxidizes siliceous, silicon
Sour aluminum, olivine matter, spinel, contains carbonaceous, contains zirconia refractory and special refractory magnesia, dolomite matter；It presses
Natural crystal and artifact can be divided into according to manufacturing method；Block elements and unshape refractory can be divided by its mode；
Not burned product, burnt product and melt-cast products can be divided into according to heat treatment mode；It can be divided into according to refractoriness common, advanced and special
Grade refractory product；Acid, neutral and basic refractory can be divided into according to chemical property；Lightweight and again can be divided into according to its density
Fire resistant materials；Standard brick, special shaped brick, special special shaped brick, pipe and flame ware can be divided into according to the shape and size of its product；Also
Blast furnace use, cement kiln use, glass furnace use, ceramic kiln refractory etc. can be divided by its application.
The poor mechanical tenacity of inorganic non-metallic material is a problem generally existing in inorganic non-metallic and material, is made
For the refractory material for belonging to inorganic non-metallic material, mechanical tenacity is also poor, although refractory material is almost in use
It does not need to be moved, but thermal shock resistance when its poor mechanical tenacity has also influenced its high temperature, in chilling urgency
Gap that is hot and using is resistance to since the influences such as cracking, peeling easily occur under the effect of expanding with heat and contract with cold for biggish temperature difference refractory material
The case where fiery material integrity, reduces the service life of refractory material；The resistance to of movement is often carried out simultaneously for those needs
Fiery material product, poor mechanical tenacity can then greatly increase the spoilage of refractory product, influence its routine use.
Summary of the invention
To solve above-mentioned purpose, the present invention provides one kind to have good mechanical toughness, while having good thermal shock resistance
The Resisting fractre refractory material of energy；
The present invention also provides a kind of preparation processes of Resisting fractre refractory material that processing step is simple and clear.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
8~10 parts of calcium of change, 6~8 parts of magnesia, 2~3 parts of manganese oxide, 3~4 parts of titanium oxide, 1~2 part of niobium pentaoxide, toughened fiber
10~15 parts.
Aluminium oxide and the inorganic oxide of silica system will form mullite phase, and mullite is a kind of with higher melt
Inorganic compound, for fusing point at 1850 DEG C or more, sieve and silica-sesquioxide system is a common and excellent refractory material system,
Simultaneous oxidation magnesium, calcium oxide are also the inorganic oxide with higher melt, reacted with sial system oxide to form solid solution can
To promote the refractoriness of refractory material, but due to the reaction temperature of the raw materials such as sial system oxide and magnesia, calcium oxide compared with
Height, so that the synthesis temperature of refractory material is higher, energy consumption is also very big, in order to not influence refractoriness or the smaller refractoriness that influences
Under the premise of suitably reduce synthesis temperature, therefore in the feed again add with reduce synthesis temperature sintering aid, manganese oxide, oxygen
Change titanium and niobium pentaoxide is some sintering aids with superperformance, can significantly be dropped in the case where a small amount of addition
The synthesis temperature of low refractory material, while the addition of these three sintering aids will not be as potassium sodium system sintering aid to fire resisting
Degree causes a large effect.
Preferably, silica is 30~35mol%, and surplus is aluminium oxide in aluminium oxide-silicon oxide mixed powder.
In sial system oxide system, the compound oikocryst that is formed when the molar percentage of silica is 30~35%
It is mutually mullite phase, mullite is that one kind has dystectic inorganic compound, and fusing point is 1850 DEG C or so, and in sial
It is that the fusing point of the compound generated when the molar percentage of silica is 30~35% is more up to 1890 in oxide system
DEG C or more, it can be at 1800 DEG C or more according to the use temperature of refractory material made from the ratio.
Preferably, silica is the silica that partial size is 95wt% or more in 200~1000nm purity, aluminium oxide is grain
Diameter is in the aluminium oxide that 200~500nm purity is 98wt% or more.
Sintering temperature also can be significantly reduced in sintering in the lesser raw material of partial size, simultaneously because partial size is small dry-pressing formed
When be easier to compress, while making the air in green body less it is sintered so that raw material is more easier to drain air in sintering
Journey faster, also makes stomata fewer, refractory material is finer and close after the completion of refractory material sintering；Material purity is bigger, then burns
The refractoriness for tying refractory material obtained is better, can be used temperature also more high.
Preferably, toughened fiber is modified zirconia fiber, it is made by following steps: the oxidation of 50 parts by weight
Zirconium, it is compound with the sodium chloride and potassium chloride of 400 parts of molar ratio 1:1 after adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight
Salt mixing after using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, calcine cool down
It ground and cleaned and dries afterwards.
Compared with sieve and silica-sesquioxide system, the mechanical tenacity of zirconium oxide is preferable, and zirconium oxide adds in the form of fibers
It is added to the toughness that refractory material can be enhanced in sieve and silica-sesquioxide refractory material；When occurring fine crack inside refractory material,
Zirconium oxide fibre inside refractory material prevents the further diffusion of crackle, realizes the purpose of enhancing refractory material toughness；
Crystal form conversion can occur when being heat-treated for zirconium oxide, and after carrying out crystal form conversion, toughening effect can be reduced, in order to prevent
This unfavorable crystal form conversion of zirconium oxide, therefore suitable calcium oxide is added to realize asking for tissue oxidizing zirconium crystal transfer
Topic, while appropriate sodium oxide molybdena is added to reduce the synthesis temperature of Zirconium oxide fibre, reduce energy consumption.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) ball milling mixing 3~5 hours, ball milling are mixed in the dehydrated alcohol of 2~3 times of raw material weights after mixing above-mentioned raw materials
By raw material stoving after conjunction；
B) will through step a, treated that raw material is dry-pressing formed under 10~20MPa pressure, refractory material green compact are made；
C) refractory material green compact after molding are sintered 3~5 hours at 1200~1400 DEG C, it is naturally cold after the completion of sintering
But to room temperature, Resisting fractre refractory material is made.
Preferably, the rotational speed of ball-mill in step a when ball milling is 1500~2000rpm.
Preferably, in step b, before dry-pressing formed, uniformly sprayed into raw material material quality 8~12% 0.1~
The aqueous sodium carbonate of 0.12mol/L and granulation.
Powder carry out it is dry-pressing formed before be granulated and make powder unity at the microballoon of 0.1mm or so, after promoting dry-pressing
Consistency, it is loose during the sintering process to be also prevented from refractory material block；Using aqueous sodium carbonate, one plays the work of granulation
With two can add suitable sodium carbonate in powder, and sodium carbonate can be decomposed at high temperature so that generating one in refractory material
A little subtle ducts, mitigate the sole mass of refractory material, can also increase the heat preservation and insulation of refractory material.
Preferably, heating rate when sintering heats up is 3~5 DEG C/min in step c.
Therefore, the invention has the following advantages:
(1) refractory material produced by the present invention mechanical tenacity with higher and good break resistance, have simultaneously
Excellent thermal shock resistance；
(2) the refractory material preparation method in the present invention is simple, is easy to be produced on existing.
Specific embodiment
Further description of the technical solution of the present invention With reference to embodiment.
Embodiment 1
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 8 parts of calcium, 6 parts of magnesia, 2 parts of manganese oxide, 3 parts of titanium oxide, 1 part of niobium pentaoxide, 10 parts of toughened fiber；Alumina-silica
In silicon mixed powder, silica 30mol%, aluminium oxide 70mol%；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 2 times of raw material weights ball milling mixing 3 hours, will after ball milling mixing
Raw material stoving；
B) will through step a, treated that raw material is dry-pressing formed under 10MPa pressure, refractory material green compact are made；
C) refractory material green compact after molding are sintered 3 hours at 1200 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made.
Embodiment 2
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 9 parts of calcium, 7 parts of magnesia, 2.5 parts of manganese oxide, 3.5 parts of titanium oxide, 1.5 parts of niobium pentaoxide, 12 parts of toughened fiber；Oxidation
In aluminium-silica mixed powder, silica 33mol%, aluminium oxide 67mol%；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 2.5 times of raw material weights ball milling mixing 4 hours, after ball milling mixing
By raw material stoving；
B) will through step a, treated that raw material is dry-pressing formed under 15MPa pressure, refractory material green compact are made；
C) refractory material green compact after molding are sintered 4 hours at 1300 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made.
Embodiment 3
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 10 parts of calcium, 8 parts of magnesia, 3 parts of manganese oxide, 4 parts of titanium oxide, 2 parts of niobium pentaoxide, 15 parts of toughened fiber；Alumina-silica
In silicon mixed powder, silica 35mol%, aluminium oxide 65mol%；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 3 times of raw material weights ball milling mixing 5 hours, will after ball milling mixing
Raw material stoving；
B) will through step a, treated that raw material is dry-pressing formed under 20MPa pressure, refractory material green compact are made；
C) refractory material green compact after molding are sintered 5 hours at 1400 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made.
Embodiment 4
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 8 parts of calcium, 6 parts of magnesia, 2 parts of manganese oxide, 3 parts of titanium oxide, 1 part of niobium pentaoxide, 10 parts of toughened fiber；Alumina-silica
In silicon mixed powder, silica 30mol%, aluminium oxide 70mol%, silica are the oxygen that partial size is 95wt% in 200nm purity
SiClx, it in 200nm purity is 98wt% aluminium oxide that aluminium oxide, which is partial size,；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 2 times of raw material weights ball milling mixing 3 hours, will after ball milling mixing
Raw material stoving；Rotational speed of ball-mill when ball milling is 1500rpm；
B) will through step a, treated that raw material is dry-pressing formed under 10MPa pressure, refractory material green compact are made；In dry-pressing
Before molding, the aqueous sodium carbonate of the 0.1mol/L of material quality 8% and granulation are uniformly sprayed into raw material；
C) refractory material green compact after molding are sintered 3 hours at 1200 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made；Heating rate when sintering heating is 3 DEG C/min.
Embodiment 5
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 8.5 parts of calcium, 7 parts of magnesia, 2 parts of manganese oxide, 3 parts of titanium oxide, 1 part of niobium pentaoxide, 12 parts of toughened fiber；Aluminium oxide-oxygen
In SiClx mixed powder, silica 32mol%, aluminium oxide 68mol%, it in 500nm purity is 97wt%'s that silica, which is partial size,
Silica, aluminium oxide are the aluminium oxide that partial size is 99wt% in 300nm purity；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 2 times of raw material weights ball milling mixing 5 hours, will after ball milling mixing
Raw material stoving；Rotational speed of ball-mill when ball milling is 200rpm；
B) will through step a, treated that raw material is dry-pressing formed under 15MPa pressure, refractory material green compact are made；In dry-pressing
Before molding, the aqueous sodium carbonate of the 0.11mol/L of material quality 10% and granulation are uniformly sprayed into raw material；
C) refractory material green compact after molding are sintered 4 hours at 1300 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made；Heating rate when sintering heating is 3 DEG C/min.
Embodiment 6
A kind of Resisting fractre refractory material, the raw material including following parts by weight: 100 parts of aluminium oxide-silicon oxide mixed powder, oxygen
Change 10 parts of calcium, 8 parts of magnesia, 3 parts of manganese oxide, 4 parts of titanium oxide, 2 parts of niobium pentaoxide, 15 parts of toughened fiber；Alumina-silica
In silicon mixed powder, silica 35mol%, aluminium oxide 65mol%, it in 1000nm purity is 99wt% oxygen that silica, which is partial size,
SiClx, it in 500nm purity is 99.9wt% aluminium oxide that aluminium oxide, which is partial size,；
Wherein, toughened fiber is modified zirconia fiber, and be made by following steps: the zirconium oxide of 50 parts by weight adds
After adding the calcium oxide of 3 parts by weight and the sodium oxide molybdena of 1 parts by weight, mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Afterwards using dehydrated alcohol as abrasive media under grind 12 hours, drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries.
A kind of preparation process of Resisting fractre refractory material, comprising the following steps:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 3 times of raw material weights ball milling mixing 5 hours, will after ball milling mixing
Raw material stoving；Rotational speed of ball-mill when ball milling is 2000rpm；
B) will through step a, treated that raw material is dry-pressing formed under 20MPa pressure, refractory material green compact are made；In dry-pressing
Before molding, the aqueous sodium carbonate of the 0.12mol/L of material quality 12% and granulation are uniformly sprayed into raw material；
C) refractory material green compact after molding are sintered 5 hours at 1400 DEG C, cooled to room temperature after the completion of sintering,
Resisting fractre refractory material is made；Heating rate when sintering heating is 5 DEG C/min.
Technical indicator:
1. refractoriness >=1860 DEG C, maximum uses temperature >=1800 DEG C；
2. apparent porosity≤5%；
3. cold crushing strength >=120MPa；
4. refractoriness under load >=1790 DEG C；
5. fracture toughness >=1.5MPam1/2。
Claims (5)
1. a kind of Resisting fractre refractory material, it is characterised in that be made of the raw material of following parts by weight: aluminium oxide-silicon oxide mixed powder
100 parts of body, 8~10 parts of calcium oxide, 6~8 parts of magnesia, 2~3 parts of manganese oxide, 3~4 parts of titanium oxide, niobium pentaoxide 1~2
Part, 10~15 parts of toughened fiber；
The toughened fiber is modified zirconia fiber, is made by following steps: the zirconium oxide of 50 parts by weight, addition 3
After the calcium oxide of parts by weight and the sodium oxide molybdena of 1 parts by weight, after being mixed with the sodium chloride and potassium chloride complex salt of 400 parts of molar ratio 1:1
Using dehydrated alcohol as abrasive media under grind 12 hours, after drying 850 DEG C temperature calcination 6 hours, ground after calcining is cooling
It cleans and dries；
In the aluminium oxide-silicon oxide mixed powder, silica is 30~35mol%, and surplus is aluminium oxide；
The silica is the silica that partial size is 95wt% or more in 200~1000nm purity, and aluminium oxide is partial size 200
~500nm purity is the aluminium oxide of 98wt% or more.
2. a kind of preparation process of Resisting fractre refractory material according to claim 1, it is characterised in that the following steps are included:
A) after above-mentioned raw materials being mixed in the dehydrated alcohol of 2~3 times of raw material weights ball milling mixing 3~5 hours, after ball milling mixing
By raw material stoving；
B) will through step a, treated that raw material is dry-pressing formed under 10~20MPa pressure, refractory material green compact are made；
C) refractory material green compact after molding are sintered 3~5 hours at 1200~1400 DEG C, are naturally cooled to after the completion of sintering
Resisting fractre refractory material is made in room temperature.
3. a kind of preparation process of Resisting fractre refractory material according to claim 2, it is characterised in that: in the step a
Rotational speed of ball-mill when ball milling is 1500~2000rpm.
4. a kind of preparation process of Resisting fractre refractory material according to claim 2, it is characterised in that: in the step b,
Before dry-pressing formed, the aqueous sodium carbonate of 0.1~0.12mol/L of material quality 8~12% is uniformly sprayed into raw material and is made
Grain.
5. a kind of preparation process of Resisting fractre refractory material according to claim 2, it is characterised in that: in the step c,
Heating rate when sintering heating is 3~5 DEG C/min.
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| CN101143783A (en) * | 2007-08-24 | 2008-03-19 | 湖南泰鑫瓷业有限公司 | Zirconium oxide plasticizing mullite ceramic material and preparation method thereof |
| CN101602605A (en) * | 2009-07-10 | 2009-12-16 | 中国地质大学（武汉） | A kind of preparation method of composite material of mullite and corundum |
| CN102272072A (en) * | 2009-01-07 | 2011-12-07 | 株式会社村田制作所 | Ceramic material for low-temperature sintering, and ceramic substrate |
| CN104311053A (en) * | 2014-10-08 | 2015-01-28 | 宁夏天纵泓光余热发电技术有限公司 | High-strength washing-resistant castable material for tundish of continuous casting machine |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101143783A (en) * | 2007-08-24 | 2008-03-19 | 湖南泰鑫瓷业有限公司 | Zirconium oxide plasticizing mullite ceramic material and preparation method thereof |
| CN102272072A (en) * | 2009-01-07 | 2011-12-07 | 株式会社村田制作所 | Ceramic material for low-temperature sintering, and ceramic substrate |
| CN101602605A (en) * | 2009-07-10 | 2009-12-16 | 中国地质大学（武汉） | A kind of preparation method of composite material of mullite and corundum |
| CN104311053A (en) * | 2014-10-08 | 2015-01-28 | 宁夏天纵泓光余热发电技术有限公司 | High-strength washing-resistant castable material for tundish of continuous casting machine |
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Address after: 313100 Meishan Town Industrial Park, Changxing County, Huzhou City, Zhejiang Province Patentee after: Zhejiang ally Refractories Co.,Ltd. Address before: 313117 Industrial Park, Changxing County Town, Changxing County, Huzhou Patentee before: CHANGXING MENGYOU REFRACTORIES Co.,Ltd. |