CN102030545A - MgAl2O4-CaAl12O19 composite-phase high-temperature resistant material and preparation method thereof - Google Patents

MgAl2O4-CaAl12O19 composite-phase high-temperature resistant material and preparation method thereof Download PDF

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CN102030545A
CN102030545A CN2010105226932A CN201010522693A CN102030545A CN 102030545 A CN102030545 A CN 102030545A CN 2010105226932 A CN2010105226932 A CN 2010105226932A CN 201010522693 A CN201010522693 A CN 201010522693A CN 102030545 A CN102030545 A CN 102030545A
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temperature resistant
resistant material
temperature
phase high
caal
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冀新友
黄朝晖
刘艳改
房明浩
张健
黄宏
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China University of Geosciences
China University of Geosciences Beijing
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China University of Geosciences Beijing
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Abstract

The invention relates to a novel MgAl2O4-CaAl12O19 composite-phase high-temperature resistant material and a preparation method thereof, belonging to the technical field of refractory materials. The composite-phase high-temperature resistant material which adopts spinel (MgAl2O4) and calcium hexaluminate (CaAl12O19) as main phases is prepared by taking a dolomite mineral and manufactured alumina as main raw materials and through the process of constituent design and regulation, binder addition, forming, sintering at high temperature in air atmosphere and the like. The main chemical compositions of the MgAl2O4-CaAl12O19 composite-phase high-temperature resistant material are Cao, Al2O3 and MgO. The invention has the characteristics of lower production cost, small density, low thermal conductivity, high corrosion resistance and high temperature resistance and good effect of heat insulation, and can be used as the high-temperature resistant material for the lining of high-temperature vessels and furnaces and the like.

Description

A kind of MgAl 2O 4-CaAl 12O 19Complex phase high-temperature resistant material and preparation method thereof
Technical field:
The present invention relates to a kind of MgAl 2O 4-CaAl 12O 19Complex phase high-temperature resistant material and preparation method thereof belongs to the refractory materials preparing technical field.
Background technology:
Along with society and expanding economy, the consumption of the energy grows with each passing day, and how rationally utilization and save energy are people's common concern and the problem that presses for solution.
Rhombspar is a calcium magnesium resource important on the earth.There are extremely abundant reserves in China, and the proven reserve at the beginning of the eighties just surpass 4,000,000,000 tons, mainly are distributed in ground such as Shandong (coastland), Shanxi, Hebei and Hubei and Hunan Provinces.Rhombspar is the important source material of producing magnesium oxide, magnesium and calcium salt, also is one of important source material of basic refractory.As the raw material of refractory materials, the importance of rhombspar is only second to magnesite, and it not only is used for steel-making converter lining, open hearth burner hearth, electric stove wall, and can be used for Thermal Equipments such as external refining device and cement kiln.In addition, rhombspar still prepares dolomite brick series (mainly contain conventional dolomite brick at present, increase zirconium white marble brick, increase zirconium konite brick etc.), the electric smelting basic raw material from refractory materialss such as marble carbon brick and electric molten magnesite rhombspar carbon bricks.
(its chemical formula is CaAl to calcium hexaluminate 12O 19Or CaO6Al 2O 3, be abbreviated as CA 6CA 6Belong to hexagonal system, have the characteristic of preferential formation sheet or platelike crystal perpendicular to the C direction of principal axis.At Al 2O 3In the refractory materialss such as the corundum-spinel the in-MgO-CaO system, aluminous cement combined corundum and alumina-magnesia castable, CA 6Thing is the reaction product under the hot conditions mutually, and the aluminium calcium that it has stronger anti-aquation and high temperature resistance slag corrosion is high temperature resistant compound, and its fusing point is 1875 ℃, is a kind of novel fire resistant material that receives much attention at present.CA 6Form of flake crystal is interspersed in the mechanical property that can improve refractory materials between corundum phase or the spinel phase.
The magnesium-aluminium spinel chemical formula is MgOAl 2O 3Or MgAl 2O 4, be called for short MA, mainly be with magnesite and MgO and Al 2O 3For feedstock production.The magnesium aluminum oxide material that MA is a kind of fusing point height (2135 ℃), good thermal shock stability, shock resistance, excellent electric insulating energy, the alkali resistant erosional competency is strong.Dolomite mineral is widely distributed in China, is the lower advantage mineral wealth of a kind of price.Particularly under situation about being becoming tight magnesite resource day now, research replaces traditional magnesite or magnesium oxide to prepare the lightening fire resistant material that contains spinel with rhombspar having great importance.
This research is that the raw material reaction in synthesizes calcium hexaluminate-spinel complex phase high-temperature resistant light material with raw mineral materials rhombspar and commercial alumina, and this preparation method not only can synthesize excellent performance MgAl cheaply 2O 4-CaAl 12O 19The complex phase high-temperature resistant light material, and this material has high temperature resistant, lightweight, thermal conductivity is low, intensity is high, heat insulation and preservation effect is good characteristics, applicable to inner lining of kiln material and elevated temperature vessel high temperature material.This research simultaneously also provides a new technological line for the comprehensive high-efficiency utilization of rhombspar mineral.
Summary of the invention:
The present invention is directed to an urgent demand of the important furnace lining material upgrading of industries of the great strategic demand of national save energy and resource and high temperature industry, research prepares the energy-conservation high temperature resistant mineral material of low-cost and high-performance with the raw mineral materials of cheapness.The use of high temperature material is that Industrial Stoves and elevated temperature vessel are realized long lifetime, low cost and one of the important measures of saving energy and reduce the cost.With widely distributed, price is lower from marble ore deposit and commercial alumina is that the synthetic a kind of novel spinel of raw material-calcium hexaluminate complex phase high-temperature resistant material can effectively utilize MgO and CaO composition in the rhombspar.The present invention is directed to the low thermal conductivity of calcium hexaluminate, under high-temperature reductibility atmosphere good stability, alkali resistant erosional competency and slag corrosion resistance ability better, feature of long life and advantage such as the magnesium-aluminium spinel resistance to elevated temperatures is good, thermal expansivity is low, propose a kind of calcium hexaluminate-spinel complex fire resistant material and preparation method thereof, thereby can effectively reach the purpose of energy-efficient, long-life hot industry inner lining of kiln of preparation and elevated temperature vessel usefulness lightening fire resistant material.
For achieving the above object, technical scheme of the present invention is as follows:
The present invention relates to a kind of MgAl 2O 4-CaAl 12O 19Complex phase high-temperature resistant material and preparation method thereof is characterized in that: described MgAl 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is mainly used in the furnace lining material of Industrial Stoves, the main thing phase composite of this high temperature material be spinel mutually with calcium hexaluminate mutually, calcium hexaluminate presents en plaque mutually, the volume density≤1.83g/cm of described high temperature material 3, ultimate compression strength 〉=26.2MPa, folding strength 〉=34.3MPa.
A kind of MgAl of the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material and preparation method thereof is characterized in that: the add-on of each raw material and specification of quality are as follows in the described preparation process: described preparation MgAl 2O 4-CaAl 12O 19Calcium source that composite diphase material is used and magnesium source are that (its specification of quality is CaCO to the dolomite mineral raw material 3MgCO 3〉=95.0%, foreign matter content＜5.0%, the particle size of raw material is 0.001～3mm); Described preparation MgAl 2O 4-CaAl 12O 19The used aluminium source raw material of composite diphase material is that (its specification of quality is Al to commercial alumina 2O 3Purity 〉=94.0%, the particle size of raw material are about 1.00mm).
A kind of MgAl of the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material, described preparation process is followed successively by: a. is a raw material with rhombspar and commercial alumina, get ground dolomite 12.0%～30.0% by mass percentage, commercial alumina powder 70.0%～88.0% mixes, add in the ball mill ball milling 0.1～24h afterwards to mixing, the mode of ball milling can be selected dry ball milling or wet ball grinding for use, ball-milling medium can be selected alumina balls or agate ball etc. for use, and the ball milling liquid that wet ball grinding is selected for use can be ethanol or water; After ball milling finishes immediately with mixed drying materials; B. the broken die for molding of packing into after outer adding additives 0～3% mixes that adds of the material of oven dry is base substrate and carries out drying that base substrate size, forming pressure and drying temperature do not have particular restriction, all can be according to conventional refractory materials processing parameter contrast; The base substrate that above-mentioned drying is good places thermal kiln furnace high temperature to burn till, and thermal kiln furnace can be electric furnace, combustion gas kiln, microwave oven, induction furnace, coal-fired kiln or oil-firing kiln.At stage insulation 10～200min of 800～1200 ℃, the temperature-rise period of other temperature does not have particular requirement in the sintering process, and final sintering temperature is 1400～1850 ℃, and insulation 0.1～40h cools to room temperature then naturally and promptly obtains MgAl of the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material.This MgAl involved in the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is a kind of have high temperature resistant, lightweight, thermal conductivity is low, intensity is high, heat insulation and preservation effect is good multiple phase refractory material.Described MgAl 2O 4-CaAl 12O 19The correlated performance index of complex phase high-temperature resistant material is: volume density≤1.83g/cm 3, ultimate compression strength 〉=26.2MPa, folding strength 〉=34.3MPa.
Description of drawings: do not have
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Raw material of the present invention is: the raw material that calcium source and magnesium source are provided is that (its specification of quality is CaCO to the dolomite mineral raw material 3MgCO 3〉=95.0%, foreign matter content＜5.0%), the particle size of raw material is 0.001～3mm; The raw material that the aluminium source is provided is commercial alumina (γ-Al 2O 3, require Al 2O 3Purity 〉=94.0wt%), the particle size of raw material is about 1.00mm.
MgAl of the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material and preparation method thereof, it is characterized in that: its preparation method is: a. is a raw material with rhombspar and commercial alumina, get ground dolomite 12.0%～30.0% by mass percentage, commercial alumina powder 70.0%～88.0% mixes, add in the ball mill ball milling 0.1～24h afterwards to mixing, the mode of ball milling can be selected dry ball milling or wet ball grinding for use, ball-milling medium can be selected alumina balls or agate ball etc. for use, and the ball milling liquid that wet ball grinding is selected for use can be ethanol or water; After ball milling finishes immediately with mixed drying materials; B. the broken die for molding of packing into after outer adding additives 0～3% mixes that adds of the material of oven dry is base substrate and carries out drying that base substrate size, forming pressure and drying temperature do not have particular restriction, all can be according to conventional refractory materials processing parameter contrast; Put into High Temperature Furnaces Heating Apparatus then, sintering under air atmosphere, sintering temperature is 1400～1850 ℃, insulation 0.1～40h cools to room temperature then naturally, wherein insulation 10～200min in 800～1200 ℃.Promptly obtain calcium hexaluminate of the present invention-spinel complex phase high-temperature resistant material, this is a kind of have high temperature resistant, lightweight, thermal conductivity is low, intensity is high, heat insulation and preservation effect is good multiple phase refractory material.
A kind of MgAl 2O 4-CaAl 12O 19Preparation technology's flow process of complex phase high-temperature resistant material is:
Raw material → batching → ball milling mixing → drying → moulding → burn till → verification test → high temperature material finished product
Embodiment 1
Raw material and proportioning:
The rhombspar specification of quality is CaCO 3MgCO 3〉=95.0%, foreign matter content＜5.0%, the particle size of raw material is 0.023mm (600 order).The specification of quality of commercial alumina is γ-Al 2O 3Purity 〉=94.0%, the particle size of raw material are about 1.00mm.Get ground dolomite 16.07% by mass percentage, commercial alumina powder 83.93% mixes.
Batching batch mixing, ball milling drying:
Mixed raw material added ball milling is to mixing in the ball mill, the ball milling time is 4h, and the mode of ball milling is selected wet ball grinding for use, and ball-milling medium is selected agate ball for use, and ball milling liquid is selected ethanol for use.Be transferred to slurry in the open container after ball milling finishes and put it into dry 12h in the baking oven,
Moulding:
The material fragmentation of oven dry caused not to be had to add the 3wt% polyvinyl alcohol after the agglomeration, moulding in the steel die of packing into after mixing, and carry out extrusion formings such as 100MPa is cold, promptly obtained base substrate.
Burn till:
The base substrate that drying is the good high temperature kiln roasting of packing into, 1500 ℃ of final firing temperatures.Calcining system is: from room temperature to 1000 ℃ 10 ℃/min of employing heat-up rate, 900 ℃ of insulation 20min by 5 ℃/min of 1000 ℃ to 1500 ℃ employings heat-up rate, to 1500 ℃ of insulation 4h, are cooled to room temperature.
The main performance index of resulting product is as follows: suitable use temperature: 1500 ℃; Volume density: 1.52g/cm 3Strength at normal temperature 34.3MPa: cold crushing strength: 26.16MPa.
Embodiment 2
Raw material and proportioning:
The rhombspar specification of quality is CaCO 3MgCO 3〉=95.0%, foreign matter content＜5.0%, the particle size of raw material is 0.023mm (600 order).The specification of quality of commercial alumina is γ-Al 2O 3Purity 〉=94.0%, the particle size of raw material are about 1.00mm.Get ground dolomite 13.00% by mass percentage, commercial alumina powder 87.00% mixes.
Batching batch mixing, ball milling drying:
Mixed raw material added ball milling is to mixing in the ball mill, the ball milling time is 6h, and the mode of ball milling is selected wet ball grinding for use, and ball-milling medium is selected agate ball for use, and ball milling liquid is selected ethanol for use.Put into baking oven and dry 12h,
Moulding:
The material fragmentation of oven dry caused not to be had to add 3wt% resol after the agglomeration, and moulding and carry out extrusion formings such as 150MPa is cold in the steel die of packing into after mixing has promptly obtained base substrate.
Burn till:
The base substrate that drying is the good high temperature kiln roasting of packing into, 1550 ℃ of final firing temperatures.Calcining system is: from room temperature to 1000 ℃ 10 ℃/min of employing heat-up rate, 900 ℃ of insulation 25min by 5 ℃/min of 1000 ℃ to 1550 ℃ employings heat-up rate, to 1550 ℃ of insulation 4h, are cooled to room temperature.
The main performance index of resulting product is as follows: suitable use temperature: 1500 ℃; Volume density: 1.63g/cm 3Strength at normal temperature 48.2MPa; Cold crushing strength: 30.16MPa.
Embodiment 3
Raw material and proportioning:
The rhombspar specification of quality is CaCO 3MgCO 3〉=95.0%, foreign matter content＜5.0%, the particle size of raw material is 0.023mm (600 order).The specification of quality of commercial alumina is γ-Al 2O 3Purity 〉=94.0%, the particle size of raw material are about 1.00mm.Get ground dolomite 10.00% by mass percentage, commercial alumina powder 90.00% mixes.
Batching batch mixing, ball milling drying:
Mixed raw material added ball milling is to mixing in the ball mill, the ball milling time is 8h, and the mode of ball milling is selected wet ball grinding for use, and ball-milling medium is selected agate ball for use, and ball milling liquid is selected ethanol for use.Put into baking oven and dry 12h,
Moulding:
The material fragmentation of oven dry caused not to be had to add the 3wt% polyvinyl alcohol after the agglomeration, and moulding and carry out extrusion formings such as 200MPa is cold in the steel die of packing into after mixing has promptly obtained base substrate.
Burn till:
The base substrate that drying is the good high temperature kiln roasting of packing into, 1600 ℃ of final firing temperatures.Calcining system is: from room temperature to 1000 ℃ 10 ℃/min of employing heat-up rate, 900 ℃ of insulation 30min by 5 ℃/min of 1000 ℃ to 1600 ℃ employings heat-up rate, to 1600 ℃ of insulation 4h, are cooled to room temperature.
The main performance index of resulting product is as follows: suitable use temperature: 1500 ℃; Volume density: 1.83g/cm 3Strength at normal temperature 52.6MPa; Cold crushing strength: 36.35MPa.

Claims (5)

1. MgAl 2O 4-CaAl 12O 19Being characterized as of complex phase high-temperature resistant material and preparation method thereof: this MgAl 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is a raw material with raw mineral materials rhombspar and commercial alumina, above-mentioned raw materials is mixed by a certain percentage and suitably adds behind the wedding agent fully mixing, prepares MgAl through technological processs such as ball milling, drying, moulding, high temperature burn till then 2O 4-CaAl 12O 19Complex phase high-temperature resistant material.
2. a kind of MgAl according to claim 1 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is characterized in that: described MgAl 2O 4-CaAl 12O 19The phase character of complex phase high-temperature resistant material is: principal crystalline phase be spinel mutually with calcium hexaluminate mutually, paracrystalline phase is the corundum phase.
3. a kind of MgAl according to claim 1 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is characterized in that: described rhombspar is commercially available raw mineral materials, and its specification of quality is CaCO 3MgCO 3〉=95.0%, foreign matter content＜5.0%, the particle size size of raw material is 0.001～3mm, its addition is that quality is from proportion by subtraction 12.0%～30.0%.
4. a kind of MgAl according to claim 1 2O 4-CaAl 12O 19Complex phase high-temperature resistant material is characterized in that: described commercial alumina is commercially available industrial raw material, and its specification of quality is Al 2O 3Purity 〉=94.0%, the particle size size of raw material is about 1.00mm, its addition is a mass percent 70.0%～88.0%.
5. a kind of MgAl according to claim 1 2O 4-CaAl 12O 19Complex phase high-temperature resistant material, described preparation process is:
A. be raw material with rhombspar and commercial alumina, take from marble dust 12.0%～30.0% by mass percentage, commercial alumina powder 70.0%～88.0% mixes, add in the ball mill ball milling 0.1～24h afterwards to mixing, the mode of ball milling can be selected dry ball milling or wet ball grinding for use, and the ball milling liquid that wet ball grinding is selected for use can be ethanol or water; After ball milling finishes immediately with mixed drying materials;
B. the broken die for molding of packing into after outer adding additives 0～3% mixes that adds of the material of oven dry is base substrate and carries out drying that base substrate size, forming pressure and drying temperature do not have particular restriction, all can be according to conventional refractory materials processing parameter contrast; The base substrate that above-mentioned drying is good places thermal kiln furnace high temperature to burn till, and thermal kiln furnace can be electric furnace, combustion gas kiln, microwave oven, induction furnace, coal-fired kiln or oil-firing kiln.At stage insulation 10～200min of 800～1200 ℃, the temperature-rise period of other temperature does not have particular requirement in the sintering process, and final sintering temperature is 1400～1850 ℃, and insulation 0.1～40h cools to room temperature then naturally and promptly obtains MgAl of the present invention 2O 4-CaAl 12O 19Complex phase high-temperature resistant material.
CN2010105226932A 2010-10-28 2010-10-28 MgAl2O4-CaAl12O19 composite-phase high-temperature resistant material and preparation method thereof Pending CN102030545A (en)

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Application publication date: 20110427