CN109734110A - A kind of alumina powder preparation method - Google Patents
A kind of alumina powder preparation method Download PDFInfo
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- CN109734110A CN109734110A CN201910149421.3A CN201910149421A CN109734110A CN 109734110 A CN109734110 A CN 109734110A CN 201910149421 A CN201910149421 A CN 201910149421A CN 109734110 A CN109734110 A CN 109734110A
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- alumina powder
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Abstract
The invention discloses a kind of alumina powder preparation methods, it is related to alumina powder preparation technical field, it is the following steps are included: step I prepares alumina powder using technical grade aluminium oxide as raw material, step II prepares the calcined alumina of small former brilliant size using the alumina powder as raw material, step III is mixed into mixed gas in the calcined alumina of small former brilliant size and carries out fumigation, step IV will it is stifling after particle be placed in low-temperature tunnel cellar and calcine, cooling obtained Reactive alumina.The alumina powder preparation method, the crystal grain of alumina powder can effectively be refined, alumina powder is set to be provided simultaneously with high-wearing feature and compression strength, PrNd alloy powder is in roasting to the refining effect of alumina grain and the perforating action of carboxymethyl cellulose, it can effectively improve micro pore shape of the alumina powder in roasting process, make alumina powder while guaranteeing advantages of higher compressive strength, itself specific surface area and Kong Rong can also be greatly improved.
Description
Technical field
The present invention relates to alumina powder preparation technical field, specially a kind of alumina powder preparation method.
Background technique
Aluminium hydroxide micro powder is a kind of environmental-protection flame-retardant filler, be mainly used in electric cable material with low smoke and halogen free, composite insulator,
The industries such as copper-clad plate and foamed material, in recent years, as national environmental protection policy constantly upgrades and industry restructuring, the country is multiple
It is swift and violent to close the development of the new industries such as insulator, wire and cable, electronic apparatus, high-speed rail and 3G/4G network, low smoke and zero halogen environmental protection is hindered
The combustion agent market demand is vigorous, and Low-smoke halogen-free environment-friendlyflame-retardant flame-retardant agent of the aluminium hydroxide micro powder as function admirable has also striden into height therewith
The track of speed development, it is not only a kind of functional material in itself, but also provides wide application prospect for the exploitation of new material,
There is extremely important effect in many fields of national economy.
In recent years, unshape refractory with high production efficiency, adaptability is good and the advantages such as material consumption is low, obtain fast
The development of speed, shared specific gravity constantly increases in refractory material, and alumina powder is as a kind of special alumina product, energy
It is enough to be dispersed in amorphous refractory well, have good water-reducing effect, anti-bleeding, it is adjustable pour setting time and
The effects of improving pouring material intensity, thus a variety of preparation methods about alumina powder have been gradually appeared in the market, however, mesh
The preparation method of preceding alumina powder is mostly towards raising product purity, reduces production cost and improve the directions such as production efficiency,
Seldom preparation method can effectively improve the alumina powder broad pore distribution uniformity, and Kong Rong, specific surface area and compression strength are high
And other effects, therefore a kind of alumina powder preparation method is needed to solve the above problems.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of alumina powder preparation method, current oxidation is solved
The preparation method of aluminium micro mist is seldom made towards improving product purity, reducing production cost and improving the directions such as production efficiency
Preparation Method can effectively improve the alumina powder broad pore distribution uniformity, Kong Rong, specific surface area and compression strength height and other effects
The problem of.
(2) technical solution
To achieve the above objectives, the technical solution adopted by the present invention is that: a kind of alumina powder preparation method, the preparation
Method the following steps are included:
Step I: using technical grade aluminium oxide as raw material, first plus pure water is modulated into uniform slurries, rear that acid solution tune is added
Section pH value is 3-5, then carries out 60-100 DEG C water bath processing 0.25-1 hours, when water-bath need to be stirred continuously, and mixing speed is
100-200r/min successively carries out slurries filtering, Washing of Filter Cake and drying after water-bath, obtain aluminium oxide filter cake.
The aluminium oxide filter cake is put into 85-95 DEG C of pure water, carried out after immersion washing until pH value be in neutrality, will
It is ground after it is dry under 120-145 DEG C of environment, obtains alumina powder.
Step II: using the alumina powder as raw material, the additive and 0.5- of first additional alumina powder 0.1-3wt%
The Organic Alcohol of 5wt%, after mixed, briquetting and drying obtain alumina block.
The alumina block is heated to 1100 DEG C -1500 DEG C with the heating rate of 6-10 DEG C/min, is calcined 1-8 hours,
It is cooled to room temperature again with 1-8 DEG C/min rate of temperature fall, the calcined alumina of small former brilliant size is made.
Step III: using the calcined alumina of the small former brilliant size as raw material, being mixed into PrNd alloy powder and three components are micro-
Powder, mist projection granulating, then filters out hydrostatic pressing of the particle through 130-150Mpa that partial size is 3-5 millimeters after mixing
Afterwards, it is put into and is passed through the mixed gas of carbon dioxide and vapor in container and carries out stifling 2-3 hours.
Step IV: the particle after will be stifling is placed in low-temperature tunnel kiln, is warming up to 40-45 DEG C per hour of heating rate
1000-1340 DEG C, 12-15 hours are kept the temperature, Reactive alumina is made after cooling.
Preferably, the calcined alumina average grain diameter of the small former brilliant size is 1-1.5 microns, and the PrNd alloy is micro-
The average grain diameter of powder is 0.5-0.7 microns, and the three components micro mist is by ZrO2, dolomite and carboxymethyl cellulose mixing and
At, and the average grain diameter of the three components micro mist is 0.6-0.8 millimeters.
Preferably, calcined alumina, PrNd alloy powder and the three component micro mists of the small former brilliant size are by weight
Ratio is 900:3:20, and ZrO in the three components micro mist2, dolomite and carboxymethylcellulocomponent component weight ratio be
2:15:3。
Preferably, the volume ratio of the carbon dioxide in gas mixture and vapor of the carbon dioxide and vapor is 1 ︰ 7.
Preferably, the acid solution is one of hydrochloric acid, sulfuric acid, acetic acid and oxalic acid or a variety of mixed liquors.
Preferably, the additive is one or both of magnesia and yttrium oxide mixture.
Preferably, the main chemical compositions of the technical grade alumina powder are as follows: Al2O3>=99.0wt%, Fe2O3≤
0.04wt%, SiO2≤ 0.04wt%, R2O≤0.12wt%, igloss≤0.80wt% and moisture≤0.50wt%, and the work
The partial size D90 of industry grade aluminum oxide powder is 38-44 microns.
(3) beneficial effect
The beneficial effects of the present invention are:
1, the alumina powder preparation method passes through the additive to alumina powder China and foreign countries plus alumina powder 0.1-3wt%
With the Organic Alcohol of 0.5-5wt%, magnesia and aluminium oxide form magnesium aluminate spinel on crystal boundary, are wrapped in the table of alumina particle
Face can effectively hinder the progress of mass transport process, and pinning crystal boundary is mobile, inhibits growing up for alumina grain, in conjunction with titanium dioxide
The suffocating treatment and PrNd alloy powder of carbon and vapor mixed gas are in sintering to the refining effect of alumina powder, energy
The effectively crystal grain of refinement alumina powder, makes alumina powder be provided simultaneously with high-wearing feature and compression strength, PrNd alloy powder is roasting
To the perforating action of the refining effect of alumina grain and carboxymethyl cellulose when burning, it can effectively improve alumina powder and roasting
Micro pore shape in the process makes alumina powder while guaranteeing advantages of higher compressive strength, can also greatly improve the ratio of itself
Surface area and Kong Rong.
2, the alumina powder preparation method, by technical grade aluminium oxide is modulated, is adjusted slurry pH value, water-bath,
Slurries filtering, Washing of Filter Cake and drying and processing, thus can effectively reduce the sodium content of raw material, while can also reduce product
Firing temperature ensure that the uniformity of product grains granularity, by using alumina powder as raw material China and foreign countries plus alumina powder 0.1-
The additive of 3wt% and the Organic Alcohol of 0.5-5wt%, thus particle surface properties can be changed, thus inhibit particle agglomeration,
Guarantee the high-ratio surface of alumina powder, meanwhile, bubbing inhibits pore to collapse in calcining, realizes hierarchical porous structure, improves
Micro mist high surface area.
3, the alumina powder preparation method, by be arranged yttrium oxide, the introducing of yttrium oxide, due to ruthenium ion size compared with
Greatly, yttrium oxide goes out to be segregated in crystal boundary, changes the chemical bond state of grain boundaries, thus can significantly inhibit alumina grain and grow up,
The calcined alumina particles of small former brilliant size can more be contributed to form by being aided with lesser heating rate and rate of temperature fall again.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of technical solution: a kind of alumina powder preparation method, and the preparation method includes following step
It is rapid:
Step I: using technical grade aluminium oxide as raw material, the main chemical compositions of the technical grade alumina powder are as follows: Al2O3≥
99.0wt%, Fe2O3≤ 0.04wt%, SiO2≤ 0.04wt%, R2O≤0.12wt%, igloss≤0.80wt% and moisture≤
0.50wt%, and the partial size D90 of the technical grade alumina powder is 38-44 microns, first plus pure water is modulated into uniform slurries,
It is 3-5 that acid solution is added afterwards and adjusts pH value, then carries out 60-100 DEG C water bath processing 0.25-1 hours, the acid solution is salt
One of acid, sulfuric acid, acetic acid and oxalic acid or a variety of mixed liquors, when water-bath, need to be stirred continuously, mixing speed 100-200r/
Min successively carries out slurries filtering, Washing of Filter Cake and drying after water-bath, obtain aluminium oxide filter cake.
The aluminium oxide filter cake is put into 85-95 DEG C of pure water, carried out after immersion washing until pH value be in neutrality, will
It is ground after it is dry under 120-145 DEG C of environment, obtains alumina powder.
Step II: using the alumina powder as raw material, the additive and 0.5- of first additional alumina powder 0.1-3wt%
The Organic Alcohol of 5wt%, the additive be one or both of magnesia and yttrium oxide mixture, after mixed, briquetting
And drying, obtain alumina block.
The alumina block is heated to 1100 DEG C -1500 DEG C with the heating rate of 6-10 DEG C/min, is calcined 1-8 hours,
It is cooled to room temperature again with 1-8 DEG C/min rate of temperature fall, the calcined alumina of small former brilliant size is made, the small former brilliant size is forged
Aluminium oxide, the ratio of PrNd alloy powder and three component micro mists by weight are burnt for 900:3:20, and in the three components micro mist
ZrO2, dolomite and carboxymethylcellulocomponent component weight ratio be 2:15:3.
Step III: using the calcined alumina of the small former brilliant size as raw material, the calcined alumina of the small former brilliant size
Average grain diameter is 1-1.5 microns, and the average grain diameter of the PrNd alloy powder is 0.5-0.7 microns, and three component is micro-
Powder is by ZrO2, dolomite and carboxymethyl cellulose mix, and the average grain diameter of the three components micro mist is 0.6-0.8 milli
Rice, is mixed into PrNd alloy powder and three component micro mists, after mixing mist projection granulating, and then filtering out partial size is 3-5 millimeters
Particle is put into after the hydrostatic pressing of 130-150Mpa and is passed through the mixed gas of carbon dioxide and vapor in container and is smoked
It steams 2-3 hours, the volume ratio of the carbon dioxide in gas mixture and vapor of the carbon dioxide and vapor is 1 ︰ 7.
Step IV: the particle after will be stifling is placed in low-temperature tunnel kiln, is warming up to 40-45 DEG C per hour of heating rate
1000-1340 DEG C, 12-15 hours are kept the temperature, Reactive alumina is made after cooling.
Below with reference to embodiment, the invention will be further described.
The average grain diameter D90 industrial aluminium hydroxide for being 38-44 microns and pure water are made into the slurries that solid content is 170g/L,
The slurries are injected into the heating water bath kettle with agitating device, it is 4 that the salt acid for adjusting pH value that concentration is 3mol/L, which is added,
Mechanical stirring speed is set as 150r/min, is heated to 80 DEG C, is carried out water bath processing 1 hour, after water bath processing, from
It so is cooled to room temperature, is filtered with centrifugal dehydrator, and is washed filter cake 3 times with hot pure water, detection pH value is neutral postposition
It is dried at a temperature of 110 DEG C；
The aluminium oxide filter cake is put into 90 DEG C of pure water, washing is carried out after immersion until pH value is in neutrality, by it
It is ground after drying under 130 DEG C of environment, obtains alumina powder, using the alumina powder as raw material, additional commercial alumina
The magnesia of powder 1.2-2wt% and the Organic Alcohol of 1.5-3wt%, mixing, briquetting, drying obtain alumina block, then by the oxygen
Change aluminium block and be heated to 1100 DEG C -1500 DEG C with the heating rate of 6-10 DEG C/min, calcines 6 hours, then with 5 DEG C/min rate of temperature fall
It is cooled to room temperature, the calcined alumina of small former brilliant size is made；
Calcined alumina, PrNd alloy powder and the three component micro mists of obtained small former brilliant size are put into after mixing
It is vacuumized in closed container, the mixed gas for then passing to carbon dioxide and vapor maintains air pressure and external pressure in container
It is equal fumigate 5 hours, wherein the weight of above-mentioned each component are as follows: the calcined alumina 1200g of small former brilliant size；PrNd is closed
Golden micro mist 6g；Three component micro mist 120g, the specific surface area for measuring the present embodiment alumina powder is 345m2/g, Kong Rongwei
0.73ml/g, compression strength are 137N/.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not limited to this hair the foregoing is merely a specific embodiment of the invention
Bright, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (7)
1. a kind of alumina powder preparation method, which is characterized in that the preparation method comprises the following steps:
Step I: using technical grade aluminium oxide as raw material, first plus pure water is modulated into uniform slurries, and the rear acid solution that is added adjusts pH
Value is 3-5, then carries out 60-100 DEG C water bath processing 0.25-1 hours, when water-bath need to be stirred continuously, mixing speed 100-
200r/min successively carries out slurries filtering, Washing of Filter Cake and drying after water-bath, obtain aluminium oxide filter cake；
The aluminium oxide filter cake is put into 85-95 DEG C of pure water, carried out after immersion washing until pH value be in neutrality, by its
It is ground after drying under 120-145 DEG C of environment, obtains alumina powder；
Step II: using the alumina powder as raw material, the first additive of additional alumina powder 0.1-3wt% and 0.5-5wt%
Organic Alcohol, after mixed, briquetting and drying obtain alumina block；
The alumina block is heated to 1100 DEG C -1500 DEG C with the heating rate of 6-10 DEG C/min, is calcined 1-8 hours, then with
1-8 DEG C/min rate of temperature fall is cooled to room temperature, and the calcined alumina of small former brilliant size is made；
Step III: using the calcined alumina of the small former brilliant size as raw material, being mixed into PrNd alloy powder and three component micro mists, mix
Then mist projection granulating after closing uniformly filters out the particle that partial size is 3-5 millimeters after the hydrostatic pressing of 130-150Mpa, is put into
The mixed gas that carbon dioxide and vapor are passed through in container fumigate 2-3 hours；
Step IV: the particle after will be stifling is placed in low-temperature tunnel kiln, is warming up to 40-45 DEG C per hour of heating rate
1000-1340 DEG C, 12-15 hours are kept the temperature, Reactive alumina is made after cooling.
2. a kind of alumina powder preparation method according to claim 1, it is characterised in that: the small former brilliant size is forged
Burning aluminium oxide average grain diameter is 1-1.5 microns, and the average grain diameter of the PrNd alloy powder is 0.5-0.7 microns, and described
Three component micro mists are by ZrO2, dolomite and carboxymethyl cellulose mix, and the average grain diameter of the three components micro mist is
0.6-0.8 millimeters.
3. a kind of alumina powder preparation method according to claim 2, it is characterised in that: the small former brilliant size is forged
Aluminium oxide, the ratio of PrNd alloy powder and three component micro mists by weight are burnt for 900:3:20, and in the three components micro mist
ZrO2, dolomite and carboxymethylcellulocomponent component weight ratio be 2:15:3.
4. a kind of alumina powder preparation method according to claim 1, it is characterised in that: the carbon dioxide and water steam
The carbon dioxide in gas mixture of gas and the volume ratio of vapor are 1 ︰ 7.
5. a kind of alumina powder preparation method according to claim 1, it is characterised in that: the acid solution be hydrochloric acid,
One of sulfuric acid, acetic acid and oxalic acid or a variety of mixed liquors.
6. a kind of alumina powder preparation method according to claim 1, it is characterised in that: the additive is magnesia
With one or both of yttrium oxide mixture.
7. a kind of alumina powder preparation method according to claim 1, it is characterised in that: the technical grade alumina powder
Main chemical compositions are as follows: Al2O3>=99.0wt%, Fe2O3≤ 0.04wt%, SiO2≤ 0.04wt%, R2O≤0.12wt%,
Igloss≤0.80wt% and moisture≤0.50wt%, and the partial size D90 of the technical grade alumina powder is 38-44 microns.
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2019
- 2019-02-28 CN CN201910149421.3A patent/CN109734110A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875132A (en) * | 2012-08-16 | 2013-01-16 | 杭州大和热磁电子有限公司 | Preparation method for large-size high-purity aluminum oxide ceramic material |
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