CN105110788B - Zircon cladding zirconium dioxide powder and preparation method thereof - Google Patents
Zircon cladding zirconium dioxide powder and preparation method thereof Download PDFInfo
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- CN105110788B CN105110788B CN201510518975.8A CN201510518975A CN105110788B CN 105110788 B CN105110788 B CN 105110788B CN 201510518975 A CN201510518975 A CN 201510518975A CN 105110788 B CN105110788 B CN 105110788B
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- zirconium dioxide
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Abstract
The present invention relates to a kind of zircon cladding zirconium dioxide powder and preparation method thereof, belong to technical field of powder engineering.Described zircon cladding zirconium dioxide powder, its kernel is monoclinic zirconium dioxide, clad is zircon, solve the problem of zircon present in existing process/zirconium oxide composite diphase material sintering densification is difficult, the sintering character of zircon/zirconium oxide composite diphase material can be effectively improved, the porosity of composite diphase material is reduced；Its preparation method includes preparing zirconium dioxide suspension, prepares coated with silica zirconium dioxide powder, prepares zircon cladding zirconium dioxide three steps of powder, and its preparation process is simple and easy to apply, it is easy to accomplish.
Description
Technical field
The present invention relates to a kind of zircon cladding zirconium dioxide powder and preparation method thereof, belong to powder technology technology neck
Domain.
Background technology
Compact zircon brick is its excellent high-temperature physical property, such as low-thermal-expansion system as the advantage of refractory material
Number, lower thermal conductivity and good corrosion resistance, can resist the erosion of glass, slag and liquid metal alloy.Compact zircon brick
As the crucial inner lining material of alkali-free glass fibre tank furnace, pool wall backing brick, bottom paving block as melting tank and depositing reservoir
With subgrade brick, the nogging of primary path and operation access, bottom brick, chute brick and wire drawing brick etc..
The main mechanism that alkali-free glass liquid is corroded it is that glass metal washes away to brick body surface, is caused by open pore
Glass metal makes short texture to brick body diffusion inside and infiltration, and brick body surface is weakened with internal bond strength, adds rushing for glass metal
Brush is acted on, outer layer brick body slow mechanism dissolved.Thus, the reduction porosity is conducive to the raising of material corrosion resistance.
Compact zircon brick the disadvantage is that, with the raising of temperature in use, under the erosion-resisting characteristics of compact zircon brick
Drop, to ensure the service life of the brick, its temperature in use is preferably below 1370 DEG C.In addition, in order that zircon brick sintering is caused
It is close, sintered usually using higher temperature or add a small amount of sintering aid, but both approaches easily cause the decomposition of zircon, make
Into short texture, and a part of christobalite phase can be produced, its anti-glass attack can be reduced.
Zirconia refractory has the aggressivity of good high temperature resistance melt, is allowed in alkali-free glass melting furnaces as contact
The inner lining material of glass metal is widely adopted.Zirconia content has more preferably for 85~95% high zirconia electrocast refractories
Corrosion resistance, low to glass feed liquid contaminative, be particularly suitable for use in low alkali and alkali-free glass melting furnaces.
Sintering oxidation Zr refractory material generally carries out all or part of stable processing, adds Y2O3, the stabilizer such as MgO, CaO
To prevent it from being burst apart because of volume excessive variation.However, this high zirconia sintered refractory containing stabilizer is used
When on glass furnace, stabilizer can be dissolved in glass metal, and stabilizing zirconia is changed into unstable zirconium oxide again, causes tissue crisp
Weak, Simultaneous Stabilization agent is combined with glass metal, can trigger in glass and the defects such as gravel, calculus occurs.In addition, zirconia material price
Height, production high-purity zirconia will significantly increase cost.
With reference to the characteristic of zircon and zirconium oxide, zircon/zirconium oxide composite diphase material research and application attract attention, according to
Its chemical composition, corrosion resistance is better than zircon material.But, due to introducing after zirconium oxide, zirconium oxide is alternate with zircon two
Agglutinating property it is poor, cause the porosity of composite diphase material higher, have impact on the raising of the anti-glass attack performance of composite diphase material.
The content of the invention
Zirconium dioxide powder is coated it is an object of the invention to provide a kind of zircon, zirconium present in existing process is solved
The problem of diamond stone/zirconium oxide composite diphase material sintering densification is difficult, can be effectively improved the burning of zircon/zirconium oxide composite diphase material
Performance is tied, the porosity of composite diphase material is reduced；Present invention simultaneously provides its preparation method.
Zircon of the present invention coats zirconium dioxide powder, and kernel is monoclinic zirconium dioxide, and clad is zircon.
Wherein：
The average grain diameter of described zirconium dioxide is in 0.1-5 μ ms；
Described zircon accounts for the 1-20wt% of powder quality, and zirconium dioxide accounts for the 80-99wt% of powder quality.
Zircon of the present invention coats zirconium dioxide raw powder's production technology, comprises the following steps：
(1) zirconium dioxide suspension is prepared：
Dispersant is dissolved in the water, its pH value is adjusted between 3-5, then adds after zirconium dioxide powder, ball milling and obtains
To the zirconium dioxide suspension of stable suspersion；
(2) coated with silica zirconium dioxide powder is prepared：
Above-mentioned zirconium dioxide suspension is stirred, acidic silicasol is added dropwise into zirconium dioxide suspension, completion of dropping is follow-up
Continuous stirring, makes sol particles absorption heat and be kept stirring on zirconium dioxide particle surface, then by suspension, makes moisture evaporation,
The zirconium dioxide powder of silica dioxide gel cladding is obtained, then it is dried, coated by titanium dioxide zirconium dioxide is obtained
Powder.
(3) zircon cladding zirconium dioxide powder is prepared：
Coated with silica zirconium dioxide powder is calcined, silica reacts with zirconium dioxide particle surface, it is raw
Into zircon be coated on zirconium dioxide particle surface, then grinding calcining after powder, obtained after sieving zircon cladding two
Zirconium powder.
Wherein：
Dispersant is modified polycarboxylic acid salt AN-2000 in step (1), with newborn acid for adjusting pH value between 3-5；Dispersant
Consumption is the 0.1-0.4wt% of zirconium dioxide powder, and the volume ratio of zirconium dioxide powder and water is 25-50:50-75, during ball milling
Between be 24-48h.
In step (2) in terms of silica, acidic silicasol addition is zirconium dioxide and silica gross mass
0.33-6.6%, is added dropwise after acidic silicasol is finished and continues to stir 4-8h；Suspension is heated to 80-90 DEG C and is kept stirring for；
Drying temperature is 200-250 DEG C, and drying time is 4-8h.
Calcining heat is 1400-1500 DEG C in step (3), and calcination time is 4-10h；Sieve mesh number is 200 mesh.
Beneficial effects of the present invention are as follows：
Zircon of the present invention coats zirconium dioxide powder, can effectively improve zircon/zirconium oxide composite diphase material
Sintering character, reduce composite diphase material the porosity；Its preparation technology is simple, it is easy to industrialized production.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
Zirconium dioxide raw material average grain diameter is 0.1 μm, and dispersant modified polycarboxylic acid salt AN-2000 consumptions are titanium dioxide zirconium powder
The volume ratio of the 0.4% of weight, zirconium dioxide powder and water is 25:75, by above-mentioned metering ratio, dispersant is dissolved in water
In, it is 5 with the pH value of newborn acid-conditioning solution, adds zirconium dioxide powder, ball milling is scattered 48 hours, obtains zirconium dioxide suspension
Liquid.
Above-mentioned suspension is stirred, acidic silicasol is slowly added dropwise, in terms of silica, addition is titanium dioxide in suspension
The 6.6% of zirconium and silica total amount.Completion of dropping, continues to stir 4 hours, suspension then is heated into 80 DEG C, stirring is dry
It is dry, then be placed in drying box 200 DEG C dry 8 hours, obtain coated with silica zirconium dioxide powder.
Above-mentioned powder is heated to 1400 DEG C in kiln, 4 hours is incubated, is down to room temperature.Powder after grinding calcining, mistake
200 mesh sieves, obtain zircon cladding zirconium dioxide powder.By metering ratio, zircon content is 20wt%.
Embodiment 2
2 μm of zirconium dioxide average grain diameter, dispersant modified polycarboxylic acid salt AN-2000 consumptions are zirconium dioxide quality
0.3%, the volume ratio of zirconium dioxide powder and water is 40:60, by above-mentioned metering ratio, dispersant is dissolved in the water, lactic acid is used
The pH value for adjusting solution is 4, adds zirconium dioxide powder, and ball milling is scattered 36 hours, obtains zirconium dioxide suspension.
Above-mentioned suspension is stirred, acidic silicasol is slowly added dropwise, in terms of silica, addition is titanium dioxide in suspension
The 3.3% of zirconium and silica total amount.Completion of dropping, continues to stir 4 hours, suspension then is heated into 85 DEG C, stirring is dry
It is dry, then be placed in drying box 220 DEG C dry 6 hours, obtain coated with silica zirconium dioxide powder.
Above-mentioned powder is heated to 1450 DEG C in kiln, 6 hours is incubated, is down to room temperature.Powder after grinding calcining, mistake
200 mesh sieves, obtain zircon cladding zirconium dioxide powder.By metering ratio, zircon content is 10wt%.
Embodiment 3
5 μm of zirconium dioxide average grain diameter, dispersant modified polycarboxylic acid salt AN-2000 consumptions are zirconium dioxide quality
0.1%, the volume ratio of zirconium dioxide powder and water is 50:50, by above-mentioned metering ratio, dispersant is dissolved in the water, lactic acid is used
The pH value for adjusting solution is 3, adds zirconium dioxide powder, and ball milling is scattered 24 hours, obtains zirconium dioxide suspension.
Above-mentioned suspension is stirred, acidic silicasol is slowly added dropwise, in terms of silica, addition is titanium dioxide in suspension
The 0.33% of zirconium and silica total amount.Completion of dropping, continues to stir 8 hours, suspension then is heated into 90 DEG C, stirring is dry
It is dry, then be placed in drying box 250 DEG C dry 4 hours, obtain coated with silica zirconium dioxide powder.
Above-mentioned powder is heated to 1500 DEG C in kiln, 10 hours is incubated, is down to room temperature.Powder after grinding calcining,
200 mesh sieves are crossed, zircon cladding zirconium dioxide powder is obtained.By metering ratio, zircon content is 1wt%.
Claims (7)
1. a kind of zircon coats zirconium dioxide raw powder's production technology, it is characterised in that：Kernel is monoclinic zirconium dioxide, cladding
Layer is zircon；
Described zircon cladding zirconium dioxide raw powder's production technology, comprises the following steps：
（1）Prepare zirconium dioxide suspension：
Dispersant modified polycarboxylic acid salt AN-2000 is dissolved in the water, lactic acid adjusts its pH value between 3-5, then adds two
The zirconium dioxide suspension of stable suspersion is obtained after Zirconium powder, ball milling；
（2）Prepare coated with silica zirconium dioxide powder：
Zirconium dioxide suspension is stirred, is added dropwise into zirconium dioxide suspension after acidic silicasol, completion of dropping and continues to stir, made
Sol particles absorption is heated and is kept stirring on zirconium dioxide particle surface, then by suspension, is made moisture evaporation, is obtained titanium dioxide
The zirconium dioxide powder of Silica hydrogel cladding, is then dried to it, obtains coated with silica zirconium dioxide powder；
（3）Prepare zircon cladding zirconium dioxide powder：
Coated with silica zirconium dioxide powder is calcined, silica reacts with zirconium dioxide particle surface, generation
Zircon is coated on zirconium dioxide particle surface, then the powder after grinding calcining, and zircon cladding titanium dioxide is obtained after sieving
Zirconium powder body；Step（3）Middle calcining heat is 1400-1500 DEG C, and calcination time is 4-10h.
2. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Zirconium dioxide
Average grain diameter in 0.1-5 μ ms.
3. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Zircon is accounted for
The 1-20 wt% of powder quality, zirconium dioxide accounts for the 80-99 wt% of powder quality.
4. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Step（1）
The consumption of middle dispersant is the 0.1-0.4 wt% of zirconium dioxide powder, and the volume ratio of zirconium dioxide powder and water is 25-50:50-
75；Ball-milling Time is 24-48h.
5. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Step（2）
In in terms of silica, acidic silicasol addition is the 0.33-6.6% of zirconium dioxide and silica gross mass, is added dropwise acid
Ludox continues to stir 4-8h after finishing.
6. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Step（2）
It is middle that suspension is heated to 80-90 DEG C and is kept stirring for；Drying temperature is 200-250 DEG C, and drying time is 4-8h.
7. zircon according to claim 1 coats zirconium dioxide raw powder's production technology, it is characterised in that：Step（3）
Middle screen cloth is 200 mesh.
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