CN109384458A - A kind of green compact calcining preparation method and applications of active alpha-alumina powder - Google Patents
A kind of green compact calcining preparation method and applications of active alpha-alumina powder Download PDFInfo
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Abstract
The present invention relates to fire resisting material fields, preparation method and applications are calcined more particularly to a kind of green compact of active alpha-alumina powder, this method includes (1) additive and raw material premix, the additive includes mineralizer and pore creating material, it counts in mass ratio, commercial alumina: mineralizer: pore creating material=95~99.5:0.05~0.5:0.5~2;The pore creating material is selected from least one of aluminium hydroxide, ammonium hydrogen carbonate, carbonate, bicarbonate, organic fiber;(2) premix adds water-wet mixed, and the moisture content of wet feed is 3~5% after mixing;(3) hydraulic brickmaking;(4) adobe is fired;(5) adobe after being burnt into obtains active alpha-alumina powder after broken through roll crushing crusher machine after ball mill grinding.The present invention makes green body while keeping structural strength, increases specific surface area, effectively discharge impurity, thermally equivalent keep the stability of α inversion of phases rate, improve product quality and stability by the way that pore creating material is added and changes the shape of adobe compression moulding.
Description
Technical field
The present invention relates to fire resisting material fields, and in particular to a kind of green compact calcining preparation method of active alpha-alumina powder
And its application.
Background technique
Alpha-alumina micro mist is one of most widely used ceramic material in various industry, its resistance to acid and alkali is strong, molding
Good, crystal phase is stablized, and hardness is high, and good stability of the dimension can be widely applied to the products such as various plastics, rubber, ceramics, refractory material
Kind, strengthening and toughening, the wearability for especially improving ceramic compactness, finish, creep resistance and high molecular material is especially shown
It writes.
The industrial production process of alpha-aluminium oxide micro mist is divided into saggar calcining and green compact calcining.It is using saggar calcined alumina
Using industrial alumina powder as raw material, it is fitted into after mixing with mineralizer in saggar and is sent into the Industrial Stoves such as tunnel oven, in high temperature
Lower transformation of crystal, it is levigate after cooling to obtain alpha-aluminium oxide micro mist.Using green compact calcined alumina be by commercial alumina, mineralizer,
It is added water and stirred after micro bonding agent is levigate together uniformly, loose adobe is pressed into using hydraulic press, is sent into tunnel after drying
Road kiln generates transformation of crystal at high temperature, broken, levigate after cooling to obtain Reactive alumina.
But the preparation method production capacity of traditional saggar calcined alumina is low, energy consumption is high;Existing green compact calcining technology exists
Following disadvantage: (1) green body is closely knit causes inside impurity when high-temperature calcination that difficulty is discharged, and it is more to burn rear impurity residual;(2) uneven heating
It is even, cause α inversion of phases rate difference big, product is unstable.
Summary of the invention
In order to overcome the above-mentioned deficiency of the prior art, the present invention provides a kind of calcinings of the green compact of active alpha-alumina powder
Preparation method and applications, the preparation method is by being added pore creating material and changing the shape of adobe compression moulding, so that green body exists
While keeping structural strength, increase specific surface area, so that impurity effectively be discharged, thermally equivalent keeps the stabilization of α inversion of phases rate
Property, improve the quality and stability of product.
To achieve the goals above, the present invention is achieved by the following technical solutions:
The first object of the present invention is to propose that a kind of green compact of active alpha alumina powder calcines preparation method, including such as
Lower step:
Step 1: additive and raw material premix: by additive and industrial alumina powder, mix preparation is premixed in proportion
Material;The additive includes mineralizer and pore creating material, is counted in mass ratio, commercial alumina: mineralizer: pore creating material=95~
99.5:0.05~0.5:0.5~2;The pore creating material is selected from aluminium hydroxide, ammonium hydrogen carbonate, carbonate, bicarbonate, organic fibre
At least one of dimension;
Step 2: premix adds water-wet mixed: premix plus water-wet are mixed, after control mixing the moisture content of wet feed be 3~
5%;
Step 3: hydraulic brickmaking: wet feed is pressed into adobe;
Step 4: adobe is fired: the adobe in step 3 is calcined 1 in 1100-1350 DEG C under the conditions of in high temperature kiln
Obtain Alpha-alumina within~8 hours;
Step 5: the adobe after firing obtains active alpha oxygen after broken through roll crushing crusher machine after ball mill grinding
Change aluminium micro mist.
Further, in the step 1 partial size of industrial alumina powder less than 100 mesh.
Further, organic fiber includes PP fiber, PVA fiber, PE fiber, appointing in PAN fiber in the step 1
It is a kind of.
Further, the mineralizer is selected from mixture or fluoride, ammonium containing boride, ammonium salt and the inorganic matter containing magnesium
The mixture of salt and the inorganic matter containing magnesium.
Further, the boride includes at least one of borax or boric acid, and fluoride includes aluminum fluoride or fluorine
Change at least one of ammonium, the ammonium salt includes at least one of ammonium chloride or ammonium fluoride, and the inorganic matter containing magnesium includes chlorine
Change at least one of magnesium or magnesium carbonate.
Further, the substance in the mineralizer by quality ratio, boride: ammonium salt: inorganic matter containing magnesium=0~
1.5:4.5~6.5:0~4.
Further, the substance in the mineralizer by quality ratio, fluoride: ammonium salt: inorganic matter containing magnesium=0~
1.5:4.5~6.5:0~4.
Further, the shape of adobe is any one of rectangular, cylindrical or porous shape in the step 3.
Further, the former grain size of the Alpha-alumina is 0.4-0.7 μm, the powder granularity of the Alpha-alumina micro mist
For D50=1.0 ± 0.05 μm.
The second object of the present invention is to propose the green compact calcining preparation method of the active alpha alumina powder of any of the above-described
Preparing the application in high-temperature refractory.
Compared with prior art, the beneficial effects of the present invention are:
1. the green compact calcining preparation method of active alpha alumina powder provided by the invention is by being added pore creating material and changing brick
The shape of base compression moulding, so that green body while keeping structural strength, increases specific surface area, so that impurity is effectively discharged,
Thermally equivalent keeps the stability of α inversion of phases rate, improves the quality and stability of product.Specifically, the pore creating material of addition not with
Aluminium oxide and additive reaction, and it is easily decomposes after heating, mistake can be burnt completely below calcination temperature and generates gas, in adobe
Micro- stomata is left, the process of gas discharge provides channel for the discharge of impurity, and effectively transmits heat, is heated evenly green body;
When hydraulic brickmaking, the shape for changing adobe compression moulding is vesicular texture, further increases the specific surface area of adobe body.
2. the green compact calcining preparation method of active alpha alumina powder of the invention is semidry method green compact calcination method, premix
When water-wet being added to mix, the moisture content of wet feed is only 3~5% after control mixing, significantly improves the load-bearing capacity of monolithic adobe and resistance to
Compressive Strength, when adobe pile being effectively prevent to fire in kiln caused by collapse;And since the wet feed moisture content of this method is extremely low,
Adobe is not necessarily to drying before firing, therefore enormously simplifies preparation flow.
3. organic fiber is added in the green compact calcining preparation method of active alpha alumina powder provided by the invention, not only have
It conducive to intensity is kept, prevents from collapsing in stacking, moreover it is possible to stomata is left after high temperature burns and loses, conducive to the discharge of impurity.
4. adobe method for cooking is simple in preparation method of the invention, calcination process can be effectively controlled, prevent burning and owe
It burns, α inversion of phases is complete, and product stability is promoted.
Specific embodiment
It shows that example illustrates certain embodiments of the present invention, and should not be construed as limiting model of the invention
It encloses.Present disclosure can be improved from material, method and reaction condition simultaneously, all these improvement should all
It falls within spirit and scope of the invention.
Embodiment 1
Containing mass ratio for 0.5 kilogram is ammonium fluoride: magnesium chloride=4.5:4 mineralizer and 950 kilograms of commercial aluminas
Powder, 5 kilograms of aluminium hydrate powders are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than 100 mesh.It will
Premix is delivered to sand mixer, and in sand mixer plus 28.67 kilograms of wet mixings of water obtain wet mixed feed.Using brick machine by wet mixed feed pressure
Rectangular adobe is made, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent into high temperature kiln in 1100
It is calcined under the conditions of~1350 DEG C and obtains within 8 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.6~0.7 μm.Brick after firing
Base obtains active alpha-alumina powder after broken through roll crushing crusher machine after ball mill grinding, Alpha-alumina micro mist
Powder granularity D50=1.0 ± 0.05 μm.
Embodiment 2
Containing mass ratio for 2.5 kilograms is boric acid: ammonium fluoride: magnesium chloride=0.75:5.25:2 mineralizer and 950 kilograms
Industrial alumina powder, 5 kilograms of ammonium hydrogen carbonate powder are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is small
In 100 mesh.Premix is delivered to sand mixer, in sand mixer plus 38.3 kilograms of wet mixings of water obtain wet mixed feed.Using brick machine
Wet mixed feed is pressed into rectangular adobe, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent to high temperature kiln
It is calcined under the conditions of 1100-1350 DEG C in furnace and obtains within 5 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.4~0.6 μm.
Adobe after firing is broken through roll crusher, and active alpha-alumina powder, alpha-oxidation are obtained after ball mill grinding after broken
Powder granularity D50=1.0 ± 0.05 μm of aluminium micro mist.
Embodiment 3
Containing mass ratio for 5 kilograms is boric acid: ammonium fluoride: magnesium chloride=1.5:6.5:4 mineralizer and 950 kilograms of industry
Alumina powder, 5 kilograms of ammonium hydrogen carbonate powder are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than
100 mesh.Premix is delivered to sand mixer, in sand mixer plus 48 kilograms of wet mixings of water obtain wet mixed feed.It will be wet using brick machine
Mixing is pressed into rectangular adobe, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent into high temperature kiln
It is calcined under the conditions of 1100-1350 DEG C and obtains within 5 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.4~0.6 μm.Firing
Adobe afterwards obtains active alpha-alumina powder, Alpha-alumina after broken through roll crushing crusher machine after ball mill grinding
Powder granularity D50=1.0 ± 0.05 μm of micro mist.
Embodiment 4
Containing mass ratio for 0.5 kilogram is boric acid: ammonium fluoride: magnesium chloride=1.5:6.5:4 mineralizer and 975 kilograms of works
Industry alumina powder, 5 kilograms of ammonium carbonate powder are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than
100 mesh.Premix is delivered to sand mixer, in sand mixer plus 39.2 kilograms of wet mixings of water obtain wet mixed feed.It will using brick machine
Wet mixed feed is pressed into rectangular adobe, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent to high temperature kiln
In calcined under the conditions of 1100-1350 DEG C and obtain within 6 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.5~0.6 μm.It burns
Adobe after obtains active alpha-alumina powder, alpha-oxidation after broken through roll crushing crusher machine after ball mill grinding
Powder granularity D50=1.0 ± 0.05 μm of aluminium micro mist.
Embodiment 5
Containing mass ratio for 0.5 kilogram is ammonium fluoride: magnesium chloride=4.5:4 mineralizer and 995 kilograms of commercial aluminas
Powder, 5 kilograms of aluminium hydrate powders are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than 100 mesh.It will
Premix is delivered to sand mixer, and in sand mixer plus 40.02 kilograms of wet mixings of water obtain wet mixed feed.Using brick machine by wet mixed feed pressure
Rectangular adobe is made, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent into high temperature kiln in 1100-
It is calcined under the conditions of 1350 DEG C and obtains within 8 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.6~0.7 μm.Adobe after firing
Through roll crushing crusher machine, active alpha-alumina powder, the powder of Alpha-alumina micro mist are obtained after ball mill grinding after broken
Body granularity D50=1.0 ± 0.05 μm.
Embodiment 6
Containing mass ratio for 0.5 kilogram is aluminum fluoride: ammonium fluoride: magnesium chloride=0.75:5.5:2 mineralizer and 950 public affairs
Jin industrial alumina powder, 15 kilograms of aluminium hydrate powders are mixed to get premix by batch mixer;The wherein grain of industrial alumina powder
Diameter is less than 100 mesh.Premix is delivered to sand mixer, in sand mixer plus 38.62 kilograms of wet mixings of water obtain wet mixed feed.Using pressure
Wet mixed feed is pressed into rectangular adobe by brick machine, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent supreme
It is calcined under the conditions of 1100-1350 DEG C in warm kiln and obtains within 6 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.5~0.6
μm.Adobe after firing obtains active alpha-alumina powder, α-after broken through roll crushing crusher machine after ball mill grinding
Powder granularity D50=1.0 ± 0.05 μm of alumina powder.
Embodiment 7
Containing mass ratio for 0.5 kilogram is aluminum fluoride: ammonium fluoride: magnesium chloride=1.5:6.5:2 mineralizer and 950 kilograms
Industrial alumina powder, 20 kilograms of PVA fibers are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than
100 mesh.Premix is delivered to sand mixer, in sand mixer plus 38.82 kilograms of wet mixings of water obtain wet mixed feed.It will using brick machine
Wet mixed feed is pressed into rectangular adobe, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent to high temperature kiln
In calcined under the conditions of 1100-1350 DEG C and obtain within 5 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.5~0.6 μm.It burns
Adobe after obtains active alpha-alumina powder, alpha-oxidation after broken through roll crushing crusher machine after ball mill grinding
Powder granularity D50=1.0 ± 0.05 μm of aluminium micro mist.
Embodiment 8
Containing mass ratio for 0.5 kilogram is aluminum fluoride: ammonium fluoride: magnesium chloride=1.5:6.5:4 mineralizer and 950 kilograms
Industrial alumina powder, 20 kilograms of PP fibers are mixed to get premix by batch mixer;Wherein the partial size of industrial alumina powder is less than
100 mesh.Premix is delivered to sand mixer, in sand mixer plus 38.82 kilograms of wet mixings of water obtain wet mixed feed.It will using brick machine
Wet mixed feed is pressed into rectangular adobe, by setting machine by adobe code base on kiln car.The kiln car for filling adobe is sent to high temperature kiln
In calcined under the conditions of 1100-1350 DEG C and obtain within 5 hours Alpha-alumina, the former grain size of Alpha-alumina is 0.5~0.6 μm.It burns
Adobe after obtains active alpha-alumina powder, alpha-oxidation after broken through roll crushing crusher machine after ball mill grinding
Powder granularity D50=1.0 ± 0.05 μm of aluminium micro mist.
Embodiment 9
Active alpha-alumina powder prepared by embodiment 1-8 and the common two kinds of active alphas-alumina powder A in market
(AMA-10) and B (AMA-20) carries out application performance comparison, and experimental result is as shown in table 1:
The Alpha-alumina micro mist of 1 embodiment 1-8 of table is compared with commercially available Alpha-alumina micro mist application performance
It is micro- by the comparing result of above-mentioned table 1 it is found that calcining preparation method using the green compact of Alpha-alumina micro mist of the invention
The α phase content of powder is up on 94.9%, and purity is up to 99% or more, significantly larger than commercially available Alpha-alumina micro mist.Therefore, of the invention
Preparation method significantly improves the quality and stability of product.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of green compact of active alpha-alumina powder calcines preparation method, characterized by the following steps:
Step 1: additive and raw material premix: by additive and industrial alumina powder, mix prepares premix in proportion;Institute
Stating additive includes mineralizer and pore creating material, is counted in mass ratio, commercial alumina: mineralizer: pore creating material=95~99.5:0.05
~0.5:0.5~2;The pore creating material in aluminium hydroxide, ammonium hydrogen carbonate, carbonate, bicarbonate, organic fiber at least
It is a kind of;
Step 2: premix adds water-wet mixed: premix plus water-wet being mixed, the moisture content of wet feed is 3~5% after control mixing;
Step 3: hydraulic brickmaking: wet feed is pressed into adobe;
Step 4: adobe is fired: by the adobe in step 3, calcining 1~8 is small in 1100-1350 DEG C under the conditions of in high temperature kiln
When obtain Alpha-alumina;
Step 5: the adobe after firing obtains active alpha-oxidation after broken through roll crushing crusher machine after ball mill grinding
Aluminium micro mist.
2. a kind of green compact of active alpha-alumina powder according to claim 1 calcines preparation method, it is characterised in that: institute
The partial size of industrial alumina powder in step 1 is stated less than 100 mesh.
3. a kind of green compact of active alpha-alumina powder according to claim 1 calcines preparation method, it is characterised in that: institute
Stating organic fiber in step 1 includes any one of PP fiber, PVA fiber, PE fiber, PAN fiber.
4. a kind of green compact of active alpha-alumina powder according to claim 1 calcines preparation method, it is characterised in that: institute
It states mineralizer and is selected from the mixed of mixture or fluoride containing boride, ammonium salt and the inorganic matter containing magnesium, ammonium salt and the inorganic matter containing magnesium
Close object.
5. a kind of green compact of active alpha-alumina powder according to claim 4 calcines preparation method, it is characterised in that: institute
Stating boride includes at least one of borax or boric acid, and the fluoride includes at least one of aluminum fluoride or ammonium fluoride,
The ammonium salt includes at least one of ammonium chloride or ammonium fluoride, the inorganic matter containing magnesium include in magnesium chloride or magnesium carbonate extremely
Few one kind.
6. a kind of green compact of active alpha-alumina powder according to claim 4 or 5 calcines preparation method, feature exists
By quality ratio in: the substance in the mineralizer, boride: ammonium salt: inorganic matter containing magnesium=0~1.5:4.5~6.5:0~4.
7. a kind of green compact of active alpha-alumina powder according to claim 4 or 5 calcines preparation method, feature exists
By quality ratio in: the substance in the mineralizer, fluoride: ammonium salt: inorganic matter containing magnesium=0~1.5:4.5~6.5:0~4.
8. a kind of green compact of active alpha-alumina powder according to claim 1 calcines preparation method, it is characterised in that: institute
The shape for stating adobe in step 3 is any one of rectangular, cylindrical or porous shape.
9. a kind of green compact of active alpha-alumina powder according to claim 1 calcines preparation method, it is characterised in that: institute
The former grain size for stating Alpha-alumina is 0.4-0.7 μm, and the powder granularity of the Alpha-alumina micro mist is D50=1.0 ± 0.05 μm.
10. the green compact calcining preparation method such as the described in any item active alpha-alumina powders of claim 1-9 is preparing high temperature
Application in refractory material.
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