CN110182834A - The preparation method and flaky alpha-alumina of flaky alpha-alumina - Google Patents
The preparation method and flaky alpha-alumina of flaky alpha-alumina Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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Abstract
A kind of preparation method and flaky alpha-alumina of flaky alpha-alumina, the preparation method of the flaky alpha-alumina use boehmite directly as silicon source to prepare flaky alpha-alumina；The Kong Rongwei 0.5ml/g-1.2ml/g of the boehmite, the specific surface area of the boehmite are 250m2/g‑360m2/g.The preparation method can reduce energy consumption, also, the flaky alpha-alumina made has the superperformance as pearlescent pigment substrate.
Description
Technical field
The invention belongs to inorganic powder material fields, are related to Alpha-alumina, and are related to them in paint (paint), industry
Coating, car paint, printing ink, the purposes in cosmetic formulations, especially as the transparent substrate of effect pigment
(substrate), more particularly, to a kind of preparation method of flaky alpha-alumina.
Background technique
The substrate of traditional pearlescent pigment, generally natural mica.Substrate of the natural mica as pearlescent pigment, need by
Screening is crushed, grinds and is classified.Due to the impurity of natural mica itself, and after grinding mica thickness and diameter it is uneven
Property, some disadvantages in traditional pearlescent pigment performance are resulted in, such as: color is not bright-coloured and color saturation is not high.With people
To pearlescent pigment require continuous improvement, it is traditional using mica as the pearlescent pigment of substrate, have been unable to meet the demand of people.
Artificial synthesized flaky alpha-alumina (Al2O3) substrate, the design freedom that can not be obtained with natural mica substrate
And physical and chemical performance.During synthesizing flaky Alpha-alumina, the introducing of impurity can be eliminated or be controlled, while has product
There are narrow particle diameter distribution and a big radius-thickness ratio, and product can be almost colourless and has smooth surface, and
And this tabular alumina has good dispersibility in water.Therefore, it is the ideal substrate of high-quality pearlescent pigment.
The preparation method of flaky alpha-alumina is varied, and most common method mainly has molten-salt growth method, high-temperature sintering process, water
Heat (alcohol heat) method, coating method, sol-gel method and Mechanical Method etc..But other than molten-salt growth method, other methods are due to sheet obtained
Alumina particle is small, and radius-thickness ratio is small, rough, bad dispersibility, substrate needed for cannot function as synthesis pearlescent pigment.
The flaky alumina of molten-salt growth method preparation has unique property.Since migration rate of the substance in fused salt is remote
Much higher than solid phase reaction, so molten-salt growth method can be significantly reduced reaction temperature and shorten the reaction time；Secondly, molten-salt growth method passes through tune
Whole fused salt amount and type, reaction temperature and time, the suitable crystal growth modifier of addition etc. can efficiently control sheet
The size and shape of aluminium oxide, can synthesize that particle diameter distribution is uniform, and radius-thickness ratio is big, the smooth tabular alumina in surface.
US5702519 has prepared flaky alumina using molten-salt growth method.This method using water-soluble inorganic aluminium salt as
Silicon source, sulfate dissolve them in a large amount of water using a small amount of phosphate and titanyl sulfate as crystal growth modifier as fused salt
Afterwards, the carbonate aqueous solution with equal chemical quantities neutralizes, and the colloidal sol of aluminium hydroxide is made, and reheats drying, sloughs a large amount of water, passes through
1200 DEG C of high temperature sintering 5h are crossed, the alumina powder of hexagonal plate structure has been prepared.Resulting this flaky alumina,
Partial size is between 3-22 μm, thickness about 200-300nm, and radius-thickness ratio is greater than 40.The method needs a large amount of water to dissolve inorganic aluminum
Salt, sulfate, carbonate and crystal growth modifier, so that subsequent drying and dehydrating process will slough a large amount of water, because before this
After be required to expend mass energy.And.It is combined unevenly between the method crystal growth modifier and aluminium hydroxide, causes crystalline substance
Body growth regulator is not high to aluminium oxide transport efficiency in fused salt, and tabular alumina partial size obtained is smaller, and particle diameter distribution is not
Uniformly, not strong as the pearlescent pigment flicker degree of substrate preparation.
US2016046812A1 discloses another method for preparing tabular alumina, and makes pearly-lustre as substrate
The method of pigment.It has equally used inorganic aluminate as silicon source, using the inorganic salts of zinc and tin as crystal growth modifier.This
Method also needs a large amount of water dissolution inorganic salts, and after obtaining alumine hydroxide colloid, needs 4 to 30 hours curing ranks
Section, energy consumption is high, and the production cycle is long.
The middle promulgated by the State Council of CN101541681A, CN1150165A, CN1936114A, CN101660204A and CN104925843A
Bright patent application, in disclosed method, big more options inorganic aluminate or compound aluminium salt are silicon source, using sodium sulphate and potassium sulfate
Mixture is fused salt, selects titanium salt, pink salt, zinc salt or phosphate for crystal growth modifier.These methods also need largely
Water, energy consumption is high, and tabular alumina partial size obtained is small, is not able to satisfy the requirement as pearlescent pigment substrate.
The preparation method for realizing the flaky alpha-alumina that a kind of water consumption is few and low energy consumption, the one kind for becoming industry need strongly
It asks, at the same time, it is desirable to which the flaky alpha-alumina of production has better performance.
Summary of the invention
Problems solved by the invention is to provide the preparation method and flaky alpha-alumina of flaky alpha-alumina.
The preparation method of flaky alpha-alumina provided by the invention prepares piece using boehmite directly as silicon source
Shape Alpha-alumina.
It is a kind of new to prepare flaky alpha-alumina rather than other aluminium oxide directly using boehmite as silicon source
Method, this flaky alpha-alumina, usual particle size is other in the micron-scale, be suitable as pearlescent pigment substrate, and
And flaky alpha-alumina prepared by corresponding preparation method provided by the invention, partial size is other in the micron-scale, and average grain diameter is big (i.e.
Size distribution D50Greatly), particle diameter distribution is uniform, and radius-thickness ratio is big, without twin, is easy the advantages that dispersing.To realize to this sheet
And partial size other Alpha-alumina in the micron-scale preparation, the present invention cooperates the following conditions and step to carry out.
In the boehmite that the present invention selects, it is preferably 0.5ml/g-1.2ml/ that the hole of the boehmite, which holds,
G, the specific surface area of the boehmite are preferably 250m2/g-360m2/g.If the Kong Rong and Bi Biao of the boehmite
Area index is less than respective range, and the crystal growth modifiers such as corresponding titanyl sulfate and sodium phosphate cannot cover to the maximum extent
Boehmite surface as much as possible is covered, the production of flaky alpha-alumina is unfavorable for.If the Kong Rong of the boehmite
It is greater than respective range with specific surface area index, illustrates its internal aperture very little, corresponding aqueous solution is not easily wetted by small aperture
Inner wall causes the crystal growth modifiers such as titanyl sulfate and sodium phosphate to be unevenly distributed, obtained final tabular alumina product
Particle diameter distribution is uneven.
Wherein, Kong Rong is often referred to the micro pore volume inside material powders particle, i.e. hole body inside unit of solid substance
Product, it is also an important indicator for measuring material activity height.The gross area possessed by specific surface area, that is, unit of solid substance
(including external surface area and endoporus area) is one of the technical indicator for indicating material activity size.
Noted earlier, corresponding preparation step is important, in the present invention, comprising the following steps:
The boehmite is dispersed in water, the first mixed liquor that mass fraction is 20%-40% is made；
Crystal growth modifier (crystal growth modifier can be solution state) is added in first mixed liquor, is made
Second mixed solution；
Second mixed solution is dried, powder is obtained；
The powder is mixed with fused salt, is calcined after the mixing, it is described calcine the temperature that uses for 1000 DEG C-
1400 DEG C, the calcining generates alpha-alumina crystal；
The alpha-alumina crystal is kept the temperature and cooled down.
In above-mentioned preparation method step, when the boehmite is dispersed in water, it is dispersed in water few as far as possible, phase
In the first mixed liquor answered, mass fraction of solids is very high.The step for, different from the first step of existing method, i.e., existing side
Method is usually that corresponding fused salt and aluminium salt are completely dissolved using a large amount of water.Method of the invention, as long as corresponding water needs are used to
Guarantee that the boehmite can scatter in water.
In above-mentioned preparation method step, when can also include at the first temperature to first mixed liquor stirring first
Between, first temperature is 60 DEG C -80 DEG C, and the first time is 15min-30min.This whipping step, in order to
Soak corresponding boehmite sufficiently.
In above-mentioned preparation method step, when can also include at the second temperature to second mixed liquor stirring second
Between, the second temperature is 20 DEG C -80 DEG C, and second time is 30min-90min.This whipping step, in order to
It is sufficiently mixed the second mixed liquor uniformly.
In above-mentioned preparation method step, the crystal growth modifier solution is that (soluble titanium salt can be with for soluble titanium salt
It is that solution state is added), the additive amount of the soluble titanium salting liquid is in terms of the quality of titanium dioxide, the quality of the titanium dioxide
Account for the 0.1%-4% of aluminum oxide quality in the boehmite.
Soluble titanium salt solution can be such as: titanyl sulfate solution, titanium tetrachloride solution or titanium trichloride solution.It can
The effect of dissolubility titanium salt solution includes the pattern and thickness for adjusting tabular alumina, to reduce twin and reunion, improves product point
Dissipate property.
Alternatively, the crystal growth modifier solution is soluble phosphate (titanium pigment in above-mentioned preparation method step
Hydrochlorate can be solution state), the additive amount of the soluble phosphoric acid salting liquid is in terms of the quality of phosphorus pentoxide, five oxidation
The quality of two phosphorus accounts for the 0.1%-3% of aluminum oxide quality in the boehmite.
Soluble phosphoric acid salting liquid is a kind of general designation, it may include that phosphate solution, metaphosphate solution or phosphoric acid are molten
Liquid etc. can be such as: sodium radio-phosphate,P-32 solution, sodium dihydrogen phosphate, sodium hexametaphosphate solution or phosphoric acid solution etc..It is soluble
When the effect of phosphate solution, the thickness of tabular alumina is reduced, improves radius-thickness ratio.Soluble phosphate is also possible to solid,
Such as sodium phosphate dodecahydrate.
Alternatively, it is also possible to simultaneously by soluble titanium salt (solution or solid) and soluble phosphate (solution or solid) conduct
The beneficial effect of the two can be superimposed by crystal growth modifier (solution or solid) at this time.
In other situations, soluble titanium salt may be the replacement of one or more of zirconates, zinc salt or pink salt etc., or
Person's crystal growth modifier is selected in one or more of titanium salt, zirconates, zinc salt and pink salt etc..
In above-mentioned preparation method step, the drying mode specifically can be drying.For example, it may be will be corresponding described
Second mixed liquor is put into the baking oven of 100 DEG C~130 DEG C (such as 120 DEG C), is dried 2-5 hours, is obtained dry powder.It can also adopt
With other drying modes, as long as moisture can be dried.In another example can be using the vacuum drying mode at 70 DEG C.
In above-mentioned preparation method step, the calcining specifically can be the fused salts such as powder and sodium sulphate and potassium sulfate, fill
Divide mixing, places into corundum crucible.Then crucible is put into Muffle furnace, is calcined at the corresponding temperature.
It is in aluminium by the above process it is found that the present invention does silicon source, also, corresponding fused salt using the boehmite
After source is mixed with crystal growth modifier, then be added in later step, in this manner it is possible to a large amount of water are saved, meanwhile, also
The energy consumed by subsequent baking step can be saved.
In above-mentioned preparation method step, the temperature used that keeps the temperature is 1000 DEG C -1400 DEG C.Soaking time can be
2h-5h.Heat preservation is to grow with allowing crystalchecked.
In above-mentioned preparation method step, the type of cooling can be natural cooling.It can also be using the cold of process control cooling
But mode, this cooling down speed can be capable of providing the environment of one slow cooling of crystal growth more slowly, and crystal can be grown
More evenly, partial size is bigger, is distributed narrower.
In above-mentioned preparation method step, the fused salt can for sodium sulphate, potassium sulfate (already described before sodium sulphate and potassium sulfate),
Sodium chloride, potassium chloride, one or more combinations of lithium sulfate, lithium chloride, sodium fluoride and potassium fluoride.
In above-mentioned preparation method step, the cooling can also be included in and washed later.Corresponding aforementioned calcination process,
Corresponding washing process may is that the product after scraping high-temperature calcination in crucible, a large amount of distilled water of the product be dissolved, so
After filter, then remove the remaining fused salt in the inside to distill water washing, insoluble matter is placed in oven drying and just obtains piece after washing
Shape Alpha-alumina.
It is silicon source that technical solution of the present invention, which directlys adopt boehmite, and boehmite, can by special selection
Preparation suitable for flaky alpha-alumina.
Meanwhile in technical solution of the present invention, using powder is first prepared, later again plus the step of corresponding fused salt, therefore,
Water consumption is few, and drying process needs dry moisture also few, and therefore, low energy consumption.
Technical solution of the present invention uses pseudo-thin diasphore with great pore volume for silicon source, intends thin water aluminium large specific surface area, therefore brilliant
Body growth regulator can more evenly be adsorbed on the aperture structure surface of boehmite, improve adjusting alpha-alumina crystals and grow up to
The efficiency of sheet.
Aforementioned preparation process is also obtained in the present invention thus and next flaky alpha-alumina, i.e. flaky alpha-alumina are using such as
The preceding preparation method preparation.The flaky alpha-alumina prepared by aforementioned preparation process, not only refers to and emphasizes monolithic sheet
Each parameter index of Alpha-alumina improves, while also more referring to the raising of the powder population parameter performance as product.
The flaky alpha-alumina size distribution D50It is 18 μm -28 μm, size distribution D50Also referred to as median diameter or grain
Spend distribution median, be 50% in cumulative distribution at particle diameter value, and be characterize pigment particle size important parameter
One of.The flaky alpha-alumina is with a thickness of 0.3 μm -0.5 μm.It follows that flaky alpha-alumina radius-thickness ratio of the invention is big.
Flaky alpha-alumina average grain diameter (size distribution D of the invention50) greatly, particle diameter distribution is uniform, and radius-thickness ratio is big, does not have
Twin is easy dispersion.
Flaky alpha-alumina provided by the invention also has the corresponding uses that can have utilization in cosmetics, such as conduct
Cosmetics functional stuffing pigment, for applying and using in decoration and personal-care supplies.
Due to the parameter and property of corresponding flaky alpha-alumina, this flaky alpha-alumina slickness is good, can be used in
The cosmetics with good skin feel are produced, and corresponding cosmetics and skin have good and lasting adhesiveness.
There can be good transparency using the filler pigments of this flaky alpha-alumina, to improve the colour of skin, cover uneven
The colour of skin, slim and graceful and natural modification is provided, realizes more natural dressing.
Granularity, thickness, draw ratio, shape, surface property and refractive index etc. influence the performance of flaky alpha-alumina.Granularity
Significantly affect coloring of the flaky alpha-alumina as filler pigments when.Granularity is smaller, and flaky alpha-alumina surface area is bigger, by
This improves coloring and enhancing is reflexive, and provides more lively color.
Flaky alpha-alumina of the invention can be used for ink, coating, preferably in car paint and plastics, and it is possible to
Containing suitable dopant, part dopant be can contribute to as the tune for granularity, thickness, optical property and configuration of surface
Agent is saved, and can inhibit the function of color that thickness is promoted to reduce and grow with particle and prevent from reuniting.
Flaky alpha-alumina of the invention can be coated with one or more metal oxide layers, wherein some metal oxygens
Compound layer can be used as high refractive index layer, and thickness depends on desired interference color.Suitable colourless low folding can also be coated with
Penetrate rate material.
Flaky alpha-alumina of the invention can also have the semi-transparent metal layer as outer layer.Metal layer can be one layer
Or multilayer.The organic dyestuff as top layer can also be coated with.
Flaky alpha-alumina of the invention can be coated with following one or more layers: TiO2Layer, Fe2O3Layer, Fe3O4Layer,
SiO2Layer, Al2O3Layer and SnO2.It can be coated by wet-chemical and (the wet-chemical painting for nacreous pigment preparation exploitation can be used
Coating method), or coated by CVD or PVD method.
Flaky alpha-alumina of the invention is used in effect pigment, suitable for all types of compositions, including plastics,
Cosmetics, and especially in automobile paint vehicle.
Flaky alpha-alumina and compatible with multiple color system based on the effect pigment of flaky alpha-alumina includes paint
Material, car paint, industrial coating, the colour system for printing ink and cosmetic formulations field.Such as intaglio plate is used in order to prepare
Printing, flexographic printing, hectographic printing and hectograph japanning printing ink, the bonding of the especially water-soluble grade of a variety of adhesives
Agent.
The form of the blend of flaky alpha-alumina of the invention and following substance uses: organic dyestuff, organic pigment or
Other pigment, such as transparent and opaque white, colour and black pigment, platelet shaped iron oxide, organic pigment, holographic face
Material, liquid crystal polymer and mica and SiO based on metal oxide-coated2Conventional transparent, the colored and black glossy of thin slice
Pigment etc..
Flaky alpha-alumina of the invention can be used for colouring coating material, agricultural plastic film, and button paste is used for kind of an attached bag
Clothing is used for food coloring, the coating of medicament or cosmetic formulations.
Flaky alpha-alumina of the invention can be used for paint vehicle and the printing ink for intaglio plate, hectograph or silk-screen printing
Adhesive composition.Such as in paint vehicle, coating, car paint, automobile covering with paint, industrial coating, paint vehicle, powdery paints, printing ink, anti-
Purposes in the preparation in the field of puppet printing ink, plastics, ceramic material.
Flaky alpha-alumina of the invention can be used in glass, paper, coating for paper, for electrophotographic printing technique
Toner, seed, greenhouse overlay film, the thermally conductive, self-supporting to insulate for machine or device, electrical isolation, in flexible sheet material, in paper and
It is used as absorbent in the laser index carving of plastics, is used as absorbent in the laser welding of plastics, contains water, organic and aqueous solvent
Graining paste in, in pigment preparation and dry preparation, such as particle, such as the clear coat in industry and automobile industry, shading
In agent, it is used as filler, especially in car paint and automobile are covered with paint, lacquer, colour wash, etc..
Detailed description of the invention
Fig. 1 is the grading curve figure of flaky alpha-alumina in embodiment one；
Fig. 2 is the grading curve figure of flaky alpha-alumina in embodiment two；
Fig. 3 is the grading curve figure of flaky alpha-alumina in embodiment three；
Fig. 4 is the grading curve figure of flaky alpha-alumina in example IV；
Fig. 5 is the grading curve figure of flaky alpha-alumina in embodiment five；
Fig. 6 is the grading curve figure of flaky alpha-alumina in embodiment six；
Fig. 7 is the stereoscan photograph figure of flaky alpha-alumina in embodiment six；
Fig. 8 is another stereoscan photograph figure of flaky alpha-alumina in embodiment six；
Fig. 9 is the grading curve figure of flaky alpha-alumina in comparative example.
Specific embodiment
The present invention provides a kind of preparation method of new flaky alpha-alumina, and provides the sheet α-being accordingly prepared
Aluminium oxide is with reference to the accompanying drawing described in detail the present invention more clearly to indicate.
Embodiment one
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 0.5ml/g of the boehmite, the specific surface area of the boehmite is 250m2/g。
Boehmite described in 22g is dispersed in 88g water, the first mixed liquor that corrresponding quality score is 25% is made；
In the first mixed liquor manufacturing process, 15min (first time) is stirred to first mixed liquor at 60 DEG C (first temperature).
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made；In the second mixing
In solution preparation process, 30min (the second time) is stirred to second mixed liquor under 60 DEG C (second temperature).
In the present embodiment, the crystal growth modifier solution is soluble titanium salting liquid, the soluble titanium salting liquid
Additive amount in terms of the quality of titanium dioxide, the quality of the titanium dioxide accounts for aluminum oxide quality in the boehmite
0.5%.Specifically, crystal growth modifier solution is aqueous solution of titanyle sulfate, the quality that concentration is 30% in the present embodiment
Percent concentration.In order to which the titanium dioxide for accounting for aluminum oxide 0.5% is added, the present embodiment is using addition 0.57g mass fraction
For 30% aqueous solution of titanyle sulfate.
Second mixed solution is dried, powder is obtained.Drying mode is drying, specifically puts the second mixed liquor
Enter and is dried in 120 DEG C of baking ovens.
The powder is mixed with fused salt, the fused salt added by the present embodiment is sodium sulphate and potassium sulfate.In the mixing
Afterwards, be put into corundum crucible, and crucible be put into Muffle furnace, calcined, the temperature that uses of calcining for 1200 DEG C,
Described to calcine the time used as 2h, the calcining generates alpha-alumina crystal.
The heat preservation and natural cooling of 2h are carried out to the alpha-alumina crystal.The temperature used that keeps the temperature is 1200 DEG C.
It is washed after the cooling.Specifically, the product after scraping high-temperature calcination in crucible, which is used
Then distilled water dissolution is filtered and is washed with distilled water, to remove the remaining fused salt in the inside, insoluble matter is placed in baking oven after washing
Drying just obtains flaky alpha-alumina.
The flaky alpha-alumina size distribution D50It is 18 μm -28 μm, with a thickness of 0.3 μm -0.5 μm.
The present invention also provides the flaky alpha-alumina using above method preparation, i.e. flaky alpha-alumina uses aforementioned preparation
Method preparation.That is the obtained flaky alpha-alumina of embodiment one, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, not twin
Crystalline substance is easy dispersion.
The flaky alpha-alumina that embodiment one obtains, using laser particle analyzer Mastersizer2000, (dispersing agent is used
Water) measurement size information, the accordingly result of measurement such as Fig. 1, i.e. Fig. 1 are that the particle diameter distribution of flaky alpha-alumina in embodiment one is bent
Line chart (particle diameter measurements curve graph), ordinate are corresponding volume (Volume) percentage composition, and abscissa is partial size ruler
Very little (Particle Size, unit are μm).
As shown in Figure 1, in the present embodiment, flaky alpha-alumina particle diameter distribution is uniform and partial size is big.Specific sheet α-oxygen
Changing aluminium relevant parameter can be in conjunction with reference to below table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 0.359 | 16.733 | 23.734 |
Table 1
In the present embodiment, size distribution D50It is 21.780 μm.
The radius-thickness ratio of product is big, is embodied in product soilless sticking and twin.
Product is easy dispersion, is embodied in when product is dispersed in water and is stirred, and can produce smooth streamline, (streamline is
When flaky powder disperses and flows in liquid, the endemism due to caused by flaky material surface reflection light).
Another easily dispersible specific manifestation of product is that corresponding flaky alpha-alumina is dispersed in coating, is carried out
Swipe, surface of the paint film obtained is smooth, and glossiness is high, no coarse granule.
Embodiment two
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 0.6ml/g of the boehmite, the specific surface area of the boehmite is 270m2/g。
Boehmite described in 22g is dispersed in 88g water, the first mixed liquor that mass fraction is 25% is made；?
In one mixed liquor manufacturing process, 20min (first time) is stirred to first mixed liquor at 65 DEG C (first temperature).
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made；In the second mixing
In solution preparation process, 35min (the second time) is stirred to second mixed liquor under 50 DEG C (second temperature).
The crystal growth modifier be soluble titanium salting liquid and soluble phosphate, the soluble titanium salting liquid and
The additive amount of soluble phosphate in terms of the quality of titanium dioxide and phosphorus pentoxide, the titanium dioxide and phosphorus pentoxide
Quality accounts for 1.5% of aluminum oxide quality in the boehmite.Specifically, soluble titanium salt uses in the present embodiment
(addition accounts for three oxidations two to the aqueous solution of titanyle sulfate and 0.45g sodium phosphate dodecahydrate solid that 1.0g mass fraction is 34.4%
The titanium dioxide and phosphorus pentoxide of aluminium 1.5%).
Second mixed solution is dried, powder is obtained, can refer to previous embodiment corresponding contents.
The powder is mixed with fused salt, in the present embodiment, the fused salt used is lithium chloride and potassium chloride.In the mixing
After calcined, the temperature that uses of calcining for 1000 DEG C, the time that the calcining uses for 5h, the calcining generation α-oxygen
Change aluminium crystal.
The alpha-alumina crystal is kept the temperature and cooled down.The temperature used that keeps the temperature keeps the temperature 5h for 1000 DEG C.
It is washed after the cooling, can refer to previous embodiment corresponding contents.
The flaky alpha-alumina that final embodiment two obtains, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, does not have
Twin is easy dispersion.
The flaky alpha-alumina that embodiment two obtains uses laser particle analyzer Mastersizer2000 (dispersing agent is water),
The accordingly result of measurement such as Fig. 2, particle diameter distribution is uniform and partial size is big.Specific flaky alpha-alumina parameter can in conjunction with reference to
Lower table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 0.315 | 19.051 | 25.810 |
Table 2
In the present embodiment, size distribution D50It is 23.447 μm.
The radius-thickness ratio of product is big, is embodied in product soilless sticking and twin.Product is easy dispersion, is embodied in and is dispersed in product
In water and when stirring, smooth streamline can produce.Another easily dispersible specific manifestation of product is, by corresponding sheet α-
Alumina dispersion carries out swipe in coating, and surface of the paint film obtained is smooth, and glossiness is high, no coarse granule.
Embodiment three
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 0.7ml/g of the boehmite, the specific surface area of the boehmite is 280m2/g。
Boehmite described in 22g is dispersed in water, the first mixed liquor that mass fraction is 25% is made；It is mixed first
It closes in liquid manufacturing process, 15min (first time) is stirred to first mixed liquor at 70 DEG C (first temperature).
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made；In the second mixing
In solution preparation process, 40min (the second time) is stirred to second mixed liquor under 40 DEG C (second temperature).
The crystal growth modifier solution is soluble titanium salting liquid, and the additive amount of the soluble titanium salting liquid is with two
The quality meter of titanium oxide, the quality of the titanium dioxide account for 0.5% of aluminum oxide quality in the boehmite.Specifically
, in the present embodiment, the soluble titanium salting liquid uses titanium tetrachloride aqueous solution, water-soluble using the titanium tetrachloride of 1.0mol/L
Liquid, and additional amount is 1.08mL.
Second mixed solution is dried, powder is obtained, with reference to previous embodiment corresponding contents.
The powder is mixed with two kinds of fused salts of lithium sulfate and lithium chloride, is calcined after the mixing, the calcining
The temperature used is 1150 DEG C, and described to calcine the time used as 4h, the calcining generates alpha-alumina crystal.
The alpha-alumina crystal is kept the temperature and cooled down.The temperature used that keeps the temperature keeps the temperature 3h for 1150 DEG C.
It is washed after the cooling, please refers to previous embodiment corresponding contents.
The flaky alpha-alumina that final embodiment one obtains, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, does not have
Twin is easy dispersion.
The present invention also provides the flaky alpha-alumina using above method preparation, i.e. flaky alpha-alumina uses aforementioned preparation
Method preparation.That is the obtained flaky alpha-alumina of embodiment three, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, not twin
Crystalline substance is easy dispersion.
The flaky alpha-alumina that embodiment three obtains, using laser particle analyzer Mastersizer2000, (dispersing agent is used
Water) measurement size information, the accordingly result of measurement such as Fig. 3.In the present embodiment, flaky alpha-alumina particle diameter distribution uniformly and partial size
Greatly.Specific flaky alpha-alumina relevant parameter can be in conjunction with reference to below table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 0.408 | 14.706 | 20.390 |
Table 3
In the present embodiment, size distribution D50It is 18.744 μm.
The radius-thickness ratio of product is big, is embodied in product soilless sticking and twin.Product is easy dispersion, is embodied in and is dispersed in product
In water and when stirring, smooth streamline can produce.Another easily dispersible specific manifestation of product is, by corresponding sheet α-
Alumina dispersion carries out swipe in coating, and surface of the paint film obtained is smooth, and glossiness is high, no coarse granule.
Example IV
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 0.8ml/g of the boehmite, the specific surface area of the boehmite is 290m2/g。
The boehmite is dispersed in water, the first mixed liquor that mass fraction is 20%-40% is made, with reference to before
State embodiment corresponding contents.
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made, with reference to aforementioned reality
Apply a corresponding contents.
The crystal growth modifier solution is soluble titanium salting liquid, and the additive amount of the soluble titanium salting liquid is with two
The quality meter of titanium oxide, the quality of the titanium dioxide account for the 0.1%-4% of aluminum oxide quality in the boehmite.
Specifically, selecting in the present embodiment using titanium tetrachloride aqueous solution as the soluble titanium salting liquid, also, additional amount calculates
For the titanium dioxide for accounting for aluminum oxide 1.0%, at this point, being the titanium tetrachloride aqueous solution that the 1.0mol/L of 2.16mL is added.
Second mixed solution is dried, powder is obtained, it is dry using vacuum drying.
The powder is mixed with fused salts such as sodium fluorides and potassium fluoride, is calcined after the mixing, the calcining is adopted
Temperature is 1250 DEG C, and described to calcine the time used as 3h, the calcining generates alpha-alumina crystal.
The alpha-alumina crystal is kept the temperature and cooled down.The temperature used that keeps the temperature keeps the temperature 2.5h for 1250 DEG C.
It is washed after the cooling, process can refer to previous embodiment corresponding contents.
The present invention also provides the flaky alpha-alumina using above method preparation, i.e. flaky alpha-alumina uses aforementioned preparation
Method preparation.That is the obtained flaky alpha-alumina of example IV, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, not twin
Crystalline substance is easy dispersion.
The flaky alpha-alumina that example IV obtains, using laser particle analyzer Mastersizer2000, (dispersing agent is used
Water) measurement size information, the accordingly result of measurement such as Fig. 4.In the present embodiment, flaky alpha-alumina particle diameter distribution uniformly and partial size
Greatly.Specific flaky alpha-alumina relevant parameter can be in conjunction with reference to below table:
Table 4
In the present embodiment, size distribution D50It is 24.508 μm.
The radius-thickness ratio of product is big, is embodied in product soilless sticking and twin.Product is easy dispersion, is embodied in and is dispersed in product
In water and when stirring, smooth streamline can produce.Another easily dispersible specific manifestation of product is, by corresponding sheet α-
Alumina dispersion carries out swipe in coating, and surface of the paint film obtained is smooth, and glossiness is high, no coarse granule.
Embodiment five
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 1.0ml/g of the boehmite, the specific surface area of the boehmite is 320m2/g。
Boehmite described in 22g is dispersed in 88g water, the first mixed liquor that mass fraction is 25% is made；?
In one mixed liquor manufacturing process, 15min (first time) is stirred to first mixed liquor at 75 DEG C (first temperature).
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made；In the second mixing
In solution preparation process, 45min (the second time) is stirred to second mixed liquor under 35 DEG C (second temperature).
The crystal growth modifier solution is soluble phosphoric acid salting liquid, the additive amount of the soluble phosphoric acid salting liquid
In terms of the quality of phosphorus pentoxide, the quality of the phosphorus pentoxide accounts for aluminum oxide quality in the boehmite
0.1%-3%.Specifically, directly plus the solid of sodium phosphate dodecahydrate, additional amount account for three in boehmite in the present embodiment
Al 2 O 0.5% (with the meter of phosphorus pentoxide in sodium phosphate dodecahydrate), it is specific that 12 hypophosphite monohydrate of 0.45g is added
Sodium.
Second mixed solution is dried, powder is obtained, can refer to previous embodiment corresponding contents.
The powder is mixed with fused salts such as potassium sulfates and potassium chloride, is calcined after the mixing, the calcining is adopted
Temperature is 1300 DEG C, and described to calcine the time used as 5h, the calcining generates alpha-alumina crystal.
The alpha-alumina crystal is kept the temperature and cooled down.The temperature used that keeps the temperature keeps the temperature 3h for 1300 DEG C.
It is washed after the cooling.
The present invention also provides the flaky alpha-alumina using above method preparation, i.e. flaky alpha-alumina uses aforementioned preparation
Method preparation.That is the obtained flaky alpha-alumina of embodiment five, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, not twin
Crystalline substance is easy dispersion.
The flaky alpha-alumina that embodiment five obtains, using laser particle analyzer Mastersizer2000, (dispersing agent is used
Water) measurement size information, the accordingly result of measurement such as Fig. 5.In the present embodiment, flaky alpha-alumina particle diameter distribution uniformly and partial size
Greatly.Specific flaky alpha-alumina relevant parameter can be in conjunction with reference to below table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 0.314 | 19.090 | 25.789 |
Table 5
In the present embodiment, size distribution D50It is 24.071 μm.
The radius-thickness ratio of product is big, is embodied in product soilless sticking and twin.Product is easy dispersion, is embodied in and is dispersed in product
In water and when stirring, smooth streamline can produce.Another easily dispersible specific manifestation of product is, by corresponding sheet α-
Alumina dispersion carries out swipe in coating, and surface of the paint film obtained is smooth, and glossiness is high, no coarse granule.
Embodiment six
A kind of preparation method of flaky alpha-alumina.
Using 22g boehmite (containing aluminum oxide 17.2g), directly as silicon source to prepare flaky alpha-alumina.
In the present embodiment, the Kong Rongwei 1.2ml/g of the boehmite, the specific surface area of the boehmite is 360m2/g。
The boehmite is dispersed in water, it is the 25% the first mixed liquors that mass fraction, which is made,；In the first mixed liquor
In manufacturing process, 30min (first time) is stirred to first mixed liquor at 80 DEG C (first temperature).
Crystal growth modifier solution is added in first mixed liquor, the second mixed solution is made；In the second mixing
In solution preparation process, 60min (the second time) is stirred to second mixed liquor under 50 DEG C (second temperature).
The crystal growth modifier solution is soluble phosphoric acid salting liquid, the additive amount of the soluble phosphoric acid salting liquid
In terms of the quality of phosphorus pentoxide, the quality of the phosphorus pentoxide accounts for aluminum oxide quality in the boehmite
1.0%.Specifically, the present embodiment directly adds the solid of sodium phosphate dodecahydrate, wiring solution-forming in advance is not had to, to reach described five
The quality for aoxidizing two phosphorus accounts for 1.0% of aluminum oxide quality in the boehmite, and 12 water of 0.90g is added in the present embodiment
Close sodium phosphate.
Second mixed solution is dried, powder is obtained.
The powder is mixed with fused salts such as sodium sulphate, potassium sulfate, sodium chloride and potassium chloride, is forged after the mixing
It burns, the temperature used of calcining is 1400 DEG C, and described to calcine the time used as 5h, it is brilliant that the calcining generates Alpha-alumina
Body.
The alpha-alumina crystal is kept the temperature and cooled down.The temperature used that keeps the temperature keeps the temperature 2h for 1400 DEG C.
It is washed after the cooling.
The present invention also provides the flaky alpha-alumina using above method preparation, i.e. flaky alpha-alumina uses aforementioned preparation
Method preparation.That is the obtained flaky alpha-alumina of embodiment six, average grain diameter is big, and particle diameter distribution is uniform, and radius-thickness ratio is big, not twin
Crystalline substance is easy dispersion.
The flaky alpha-alumina that embodiment six obtains, using laser particle analyzer Mastersizer2000, (dispersing agent is used
Water) measurement size information, the accordingly result of measurement such as Fig. 6.In the present embodiment, flaky alpha-alumina particle diameter distribution uniformly and partial size
Greatly.Specific flaky alpha-alumina relevant parameter can be in conjunction with reference to below table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 0.306 | 19.614 | 28.584 |
Table 6
In the present embodiment, size distribution D50It is 26.341 μm.
Referring to Figure 7, show the part partial size stereoscan photograph of flaky alpha-alumina manufactured in the present embodiment,
Therefrom it can be seen that, flaky alpha-alumina particle diameter distribution (size distribution) is in the level more understood and (shows 13.98 in figure
μm, 7.26 μm and 28.52 μm of three partial sizes).
Referring to Figure 8, show the stereoscan photograph of flaky alpha-alumina segment thickness manufactured in the present embodiment,
Therefrom show flaky alpha-alumina (shows 0.332 μm and 0.327 μm of two thickness with a thickness of 0.3 μm -0.5 μm in figure
Degree).
It can see in conjunction with Fig. 7 and Fig. 8, the radius-thickness ratio for the product that the present embodiment obtains is big, product soilless sticking and twin.
Product is easy dispersion, is embodied in when product is dispersed in water and is stirred, and can produce smooth streamline.Product holds
Another specific manifestation easily dispersed is that corresponding flaky alpha-alumina is dispersed in coating, carries out swipe, paint film obtained
Surface is smooth, and glossiness is high, no coarse granule.
Some steps between various embodiments of the present invention can cross-referenced and replacement.
Comparative example
The preparation of solution A: 111.9g Patent alum (containing aluminium oxide 17.2g) is used as silicon source, water-soluble with 300g
Solution, and 57.3g sodium sulphate and 46.9g potassium sulfate is added, and 34.4% aqueous solution of titanyle sulfate of 1.0g is added, at 60 DEG C
Stirring, until being completely dissolved.
The preparation of B solution: 150g water is added in 54g natrium carbonicum calcinatum, 12 water of 0.45g and sodium phosphate, and heating stirring is molten
Solution.
B solution is toward being added dropwise in solution A, after adding, by white colloidal or suspension drying moisture (it follows that above-mentioned body
At least 504g water in system, the pact in the about 450g water and Patent alum that add when being prepared including solution A and B solution
54g water), obtain powder, powder also passes through calcining, calcines the temperature used as 1200 DEG C, it is described calcine time for using for
4h, the calcining generate alpha-alumina crystal.The alpha-alumina crystal is kept the temperature and cooled down.The temperature that the heat preservation uses
Degree is 1200 DEG C, keeps the temperature 4h.
Finally obtained flaky alpha-alumina is surveyed using laser particle analyzer Mastersizer2000 (dispersing agent uses water)
Size information is measured, the accordingly result of measurement such as Fig. 9 sees from the curve in Fig. 9, and particle diameter distribution is uneven, and the body that partial size is small
Product accounting is larger.Specific flaky alpha-alumina relevant parameter can be in conjunction with reference to below table:
| Specific surface area (m2/g) | Surface area average grain diameter (μm) | Volume average particle size (μm) |
| 1.07 | 5.610 | 20.373 |
Table 7
In comparative example, size distribution D50It is 16.203 μm, less than 18 μm, also, the radius-thickness ratio of product and dispersibility are not
Such as foregoing embodiments.
Embodiment one to six and above-mentioned comparative example are compared it is found that equally will be containing 17.2g aluminum oxide
Silicon source is used to make flaky alpha-alumina, and the water consumption of various embodiments of the present invention substantially reduces, dry needed for corresponding drying process
Moisture also accordingly tail off, therefore, method energy consumption of the invention is lower.Meanwhile various embodiments of the present invention are all made of macropore appearance and intend
Boehmite is silicon source, intends thin water aluminium large specific surface area, therefore crystal growth modifier can more evenly be adsorbed on and intend thin water aluminium
The aperture structure surface of stone improves the efficiency for adjusting the long slabbing of alpha-alumina crystals, ensure that each embodiment is finally obtained
Flaky alpha-alumina average grain diameter (size distribution D50) greatly, particle diameter distribution is uniform, and radius-thickness ratio is big, without twin, is easy dispersion, i.e.,
The flaky alpha-alumina that the embodiment of the present invention obtains has the superperformance as pearlescent pigment substrate.
Although present disclosure is as above, present invention is not limited to this.Anyone skilled in the art are not departing from this
It in the spirit and scope of invention, can make various changes or modifications, therefore protection scope of the present invention should be with claim institute
Subject to the range of restriction.
Claims (10)
1. a kind of preparation method of flaky alpha-alumina, which is characterized in that use boehmite directly as silicon source to prepare
Flaky alpha-alumina；The Kong Rongwei 0.5ml/g-1.2ml/g of the boehmite, the specific surface area of the boehmite are
250m2/g-360m2/g。
2. the preparation method of flaky alpha-alumina as described in claim 1, which comprises the following steps:
The boehmite is dispersed in water, the first mixed liquor that mass fraction is 20%-40% is made；
Crystal growth modifier is added in first mixed liquor, the second mixed solution is made；
Second mixed solution is dried, powder is obtained；
The powder is mixed with fused salt, is calcined after the mixing, the temperature used of calcining is 1000 DEG C -1400
DEG C, described to calcine the time used as 2h-5h, the calcining generates alpha-alumina crystal；
The alpha-alumina crystal is kept the temperature and cooled down.
3. the preparation method of flaky alpha-alumina as claimed in claim 2, which is characterized in that further include right at the first temperature
At the first time, first temperature is 60 DEG C -80 DEG C for the first mixed liquor stirring, and the first time is 15min-30min.
4. the preparation method of flaky alpha-alumina as claimed in claim 3, which is characterized in that further include right at the second temperature
Second mixed liquor stirred for the second time, and the second temperature is 20 DEG C -80 DEG C, and second time is 30min-90min.
5. the preparation method of flaky alpha-alumina as claimed in claim 2, which is characterized in that it is described keep the temperature the temperature that uses for
1000℃-1400℃。
6. the preparation method of flaky alpha-alumina as claimed in claim 2, which is characterized in that
The crystal growth modifier is soluble titanium salt, the additive amount of the solubility titanium salt in terms of the quality of titanium dioxide,
The quality of the titanium dioxide accounts for the 0.1%-4% of aluminum oxide quality in the boehmite；
Alternatively, the crystal growth modifier is soluble phosphate, the additive amount of the soluble phosphate is with five oxidations two
The quality meter of phosphorus, the quality of the phosphorus pentoxide account for the 0.1%-3% of aluminum oxide quality in the boehmite.
7. the preparation method of flaky alpha-alumina as claimed in claim 2, which is characterized in that the fused salt is sodium sulphate, sulphur
Sour potassium, sodium chloride, potassium chloride, one or more combinations of lithium sulfate, lithium chloride, sodium fluoride and potassium fluoride.
8. the preparation method of flaky alpha-alumina as claimed in claim 2, which is characterized in that further include after the cooling
It is washed.
9. a kind of flaky alpha-alumina, which is characterized in that using the preparation method system as described in claim 1-8 any one
It is standby.
10. flaky alpha-alumina as claimed in claim 9, which is characterized in that the size distribution D of the flaky alpha-alumina50
It is 18 μm -28 μm, with a thickness of 0.3 μm -0.5 μm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021068139A1 (en) * | 2019-10-09 | 2021-04-15 | Dic Corporation | Alumina particles and method for producing alumina particles |
| KR102302448B1 (en) * | 2021-01-12 | 2021-09-16 | 주식회사 티세라 | Plate-shaped α-alumina particles and method thereof |
| CN114920272A (en) * | 2022-05-27 | 2022-08-19 | 贵阳职业技术学院 | Method for rapidly preparing flaky alumina |
| JP2022550984A (en) * | 2019-10-09 | 2022-12-06 | Dic株式会社 | Composite particles and method for producing the composite particles |
| JP2022550986A (en) * | 2019-10-09 | 2022-12-06 | Dic株式会社 | Composite particles and method for producing composite particles |
| JP2022551131A (en) * | 2019-10-09 | 2022-12-07 | Dic株式会社 | Plate-like alumina particles and method for producing plate-like alumina particles |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150165A (en) * | 1995-09-14 | 1997-05-21 | 默克专利股份有限公司 | Flaky aluminium oxide and pearlescent pigment, and production thereof |
| WO2006101306A1 (en) * | 2005-03-25 | 2006-09-28 | Korea Research Institute Of Chemical Technology | Flaky alpha-alumina crystal and a method of its preparation |
| CN101541681A (en) * | 2006-08-28 | 2009-09-23 | 韩国化学研究院 | Flaky alpha-alumina crystals with large aspect ratio and a preparation method of the same |
| CN103359764A (en) * | 2013-07-09 | 2013-10-23 | 东华大学 | Preparation method of sheet-shaped alpha-aluminium oxide |
| US20140322536A1 (en) * | 2013-04-30 | 2014-10-30 | Merck Patent Gmbh | Alpha-alumina flakes |
| CN104986786A (en) * | 2015-07-31 | 2015-10-21 | 华南理工大学 | Sheet alpha-Al2O3 powder body with controllable particle diameter size and preparation method of sheet alpha-Al2O3 powder body |
| CN105645445A (en) * | 2016-01-06 | 2016-06-08 | 成都理工大学 | Platy-monocrystal alpha-aluminum oxide, and preparation method and application thereof |
-
2019
- 2019-05-30 CN CN201910466121.8A patent/CN110182834B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150165A (en) * | 1995-09-14 | 1997-05-21 | 默克专利股份有限公司 | Flaky aluminium oxide and pearlescent pigment, and production thereof |
| WO2006101306A1 (en) * | 2005-03-25 | 2006-09-28 | Korea Research Institute Of Chemical Technology | Flaky alpha-alumina crystal and a method of its preparation |
| CN101541681A (en) * | 2006-08-28 | 2009-09-23 | 韩国化学研究院 | Flaky alpha-alumina crystals with large aspect ratio and a preparation method of the same |
| US20140322536A1 (en) * | 2013-04-30 | 2014-10-30 | Merck Patent Gmbh | Alpha-alumina flakes |
| CN103359764A (en) * | 2013-07-09 | 2013-10-23 | 东华大学 | Preparation method of sheet-shaped alpha-aluminium oxide |
| CN104986786A (en) * | 2015-07-31 | 2015-10-21 | 华南理工大学 | Sheet alpha-Al2O3 powder body with controllable particle diameter size and preparation method of sheet alpha-Al2O3 powder body |
| CN105645445A (en) * | 2016-01-06 | 2016-06-08 | 成都理工大学 | Platy-monocrystal alpha-aluminum oxide, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| ZHU LI-HUI ET AL.: ""Morphology control of α-Al2O3 platelets by molten salt synthesis"", 《CERAMICS INTERNATIONAL》 * |
| 张倩影 等: ""添加剂在熔盐法合成片状α-Al2O3中的作用"", 《材料研究学报》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021068139A1 (en) * | 2019-10-09 | 2021-04-15 | Dic Corporation | Alumina particles and method for producing alumina particles |
| CN114555718A (en) * | 2019-10-09 | 2022-05-27 | Dic株式会社 | Alumina particles and method for producing alumina particles |
| JP2022550984A (en) * | 2019-10-09 | 2022-12-06 | Dic株式会社 | Composite particles and method for producing the composite particles |
| JP2022550986A (en) * | 2019-10-09 | 2022-12-06 | Dic株式会社 | Composite particles and method for producing composite particles |
| JP2022550985A (en) * | 2019-10-09 | 2022-12-06 | Dic株式会社 | Alumina particles and method for producing alumina particles |
| JP2022551131A (en) * | 2019-10-09 | 2022-12-07 | Dic株式会社 | Plate-like alumina particles and method for producing plate-like alumina particles |
| JP7388548B2 (en) | 2019-10-09 | 2023-11-29 | Dic株式会社 | Alumina particles and method for producing alumina particles |
| JP7388549B2 (en) | 2019-10-09 | 2023-11-29 | Dic株式会社 | Composite particles and method for producing composite particles |
| CN114555718B (en) * | 2019-10-09 | 2024-01-26 | Dic株式会社 | Alumina particles and method for producing alumina particles |
| KR102302448B1 (en) * | 2021-01-12 | 2021-09-16 | 주식회사 티세라 | Plate-shaped α-alumina particles and method thereof |
| WO2022154227A1 (en) * | 2021-01-12 | 2022-07-21 | 주식회사 티세라 | Plate type α-alumina and manufacturing method therefor |
| CN114920272A (en) * | 2022-05-27 | 2022-08-19 | 贵阳职业技术学院 | Method for rapidly preparing flaky alumina |
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