CN109650423A - A kind of polymolecularity flaky alpha-alumina raw powder's production technology - Google Patents
A kind of polymolecularity flaky alpha-alumina raw powder's production technology Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01F7/00—Compounds of aluminium
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- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
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Abstract
The present invention relates to a kind of polymolecularity flaky alpha-alumina raw powder's production technologies.The present invention by preparation containing silicon source, fused salt, chemical additives suspension a, solution b containing carbonate, dispersing agent, solution b is added in suspension a with certain rate and is uniformly mixed with magnetic stirring apparatus with certain revolving speed, stirring drying calcining after a certain period of time, fused salt is washed with deionized water, then is freeze-dried to obtain the flaky alpha-alumina powder of polymolecularity, complete hexagonal.The present invention can be made particle diameter distribution uniformly, soilless sticking high dispersive, radius-thickness ratio be small, regular shape is in hexagonal flaky alpha-alumina.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of polymolecularity flaky alpha-alumina raw powder's production technology.
Background technique
Flaky alpha-alumina is a kind of special construction of aluminium oxide, not only has that the anti-oxidant of aluminium oxide, fusing point be high, corrosion resistant
Erosion, the features such as thermal conductivity is good, but also have good adhesion, certain surface-active, easily dispersion, to the reflection energy of light
Power and excellent screen effect, are used in the fields such as pearlescent pigment, refractory material, cosmetics, automobile finish, have huge
Application value.
Currently, the preparation method of flaky alpha-alumina mainly has hydro-thermal method, Mechanical Method, coating method, molten-salt growth method, gel-combustion
Burning method etc..Wherein the flaky alpha-alumina particle diameter distribution of molten-salt growth method preparation is uniform, and radius-thickness ratio is big, and the additive being added makes piece
Shape Alpha-alumina controllability is strong, and fabulous meets the needs of every field.It is described in patent CN105731509 and a kind of prepares piece
Then the method for shape Alpha-alumina, the method are passed through each raw material by preparing aluminium salt, titanium salt, sodium salt, phosphate and basic materials
Organic solvent assists ball milling to be uniformly mixed, and is calcined, is cooled to room temperature after drying, flaky alpha-alumina is obtained after purification.It should
The flaky alpha-alumina partial size of method preparation changes in gradient, but does not account for flaky alpha-alumina uniform particle sizes' degree.Patent
Provide a kind of flaky alpha-alumina powder and preparation method thereof in CN107140666, the method is by nm boehmite, fluoride mine
Agent and dehydrated alcohol ball milling, obtain mixed material, and the mixed material and fused salt mixed calcining are obtained flaky alpha-alumina.
Because fluoride there can be very big difference in structure, but it is difficult to control the toxicity of fluoride mineral agent, to cause to people
The non-intellectual that body and environment influence, and prepared flaky alpha-alumina partial size is smaller, and thickness is larger.Above-mentioned patent is deposited respectively
It affects in the big unfavorable factor of energy consumption and to human body, environment, the flaky alpha-alumina radius-thickness ratio of preparation is also paid no attention to
Think.And after fused salt is washed with deionized water in flaky alpha-alumina made from molten-salt growth method, drying will cause flaky alpha-alumina company
It is connected into block, if being formed into powder, during grinding flaky alpha-alumina hexagonal configuration can destroy, can also make sheet α-oxygen
The dispersibility for changing aluminium reduces.These problems all restrict the development of flaky alpha-alumina preparation.
Summary of the invention
It is an object of the invention to overcome molten-salt growth method of the existing technology prepare partial size not enough uniformly, radius-thickness ratio not enough manages
Think, the defect that hexagonal plate Alpha-alumina is sufficiently complete, a kind of polymolecularity flaky alpha-alumina raw powder's production technology is provided.
The present invention by preparation containing silicon source, fused salt, chemical additives suspension a, the solution b containing carbonate, dispersing agent, will be molten
Liquid b is added in suspension a and is uniformly mixed with certain rate, and stirring drying calcining after a certain period of time is washed with deionized water
Fused salt is removed, then is freeze-dried to obtain the flaky alpha-alumina powder of polymolecularity, complete hexagonal.Partial size can be made by the method
It is evenly distributed, soilless sticking, high dispersive, radius-thickness ratio are small, regular shape is in hexagonal flaky alpha-alumina.
The purpose of the invention is achieved by the following technical solution:
A kind of polymolecularity flaky alpha-alumina raw powder's production technology, includes the following steps:
(1) deionized water is added to stir and evenly mix silicon source, fused salt, chemical additives to obtain suspension a；
(2) deionized water is added to be uniformly mixed carbonate, dispersing agent to obtain solution b；
(3) the solution b of mixing is added in suspension a with certain rate, stirs and evenly mixs drying；
(4) by the gel mixture of drying with suitable temperature calcination, with being freeze-dried after deionized water rinse solution
To polymolecularity flaky alpha-alumina.
Silicon source described in step (1) is one of aluminum sulfate octadecahydrate, aluminium chloride, the object of aluminium element in source of aluminium
The ratio between amount and the amount of substance of fused salt of matter are 1:(2~5)；
Fused salt described in step (1) is Na2SO4–K2SO4, one of NaCl-KCl, wherein mole of fused salt and aluminium salt
Concentration is than preferred 3:1-5:1；
Chemical additives described in step (1) are SiO2、TiO2、MnO2, one or more of ZnO etc., wherein crystal form control
The quality of preparation is to convert available Al relative to by silicon source2O3Quality 0.5% -4%.
Carbonate described in step (2) be sodium carbonate, sodium bicarbonate, potassium carbonate, in saleratus any one or it is several
Kind, wherein the amount of added carbonate makes it carry out completely double hydrolysis or excess with aluminium salt；
Dispersing agent described in step (2) is Na3PO4, additional amount is to convert available Al relative to by silicon source2O3Matter
The 0.5% -4% of amount.
It is 0.001mol/min- that carbonate, which is added to the rate in suspension a, in control solution b described in step (3)
0.45mol/min。
Drying temperature described in step (3) is preferably 60 DEG C -80 DEG C.
Calcination temperature described in step (4) is 900 DEG C -1200 DEG C, and the time for rising to calcination temperature from room temperature is 200min -
400min, sintering soak time are 4h -6h.
Deionized water wash number described in step (4) is preferably 3-4 times；The freeze-drying temperature is preferably -70
DEG C-- 80 DEG C, sublimation drying is preferably 2-10h；
The amount of deionized water is completely dissolved silicon source in step (1), and stirring rate is 200r/min -350r/
Min, mixing time are 30min -40min.
The type and dosage, the dosage of dispersing agent, mixing time, calcining that the present invention passes through control fused salt, chemical additives
Temperature controls flaky alpha-alumina radius-thickness ratio.The rate control piece of carbonate in the solution b of suspension a is added to by controlling
The uniformity and radius-thickness ratio of shape Alpha-alumina, in certain addition velocity interval, the addition speed of carbonate is faster, reaction speed
Rate is faster, but the too fast generation that will lead to carbon dioxide bubble of rate is more violent, influences the pattern of α tabular alumina.It is logical
Cross the dispersibility of freeze-drying control flaky alpha-alumina.The method controllability is extremely strong, can obtain high dispersive and radius-thickness ratio is in ladder
Spend the flaky alpha-alumina powder of distribution.Compared with prior art, the invention has the advantages that and significant progress:
(1) it controls carbonate in solution b and is added to the rate in suspension a, control reaction rate, obtained piece
Shape Alpha-alumina partial size is bigger, and radius-thickness ratio is smaller, and particle diameter distribution is more uniform；
(2) sintering temperature can significantly be effectively reduced by chemical additives being added, and control the dosage and type of chemical additives
It can control flaky alpha-alumina pattern and radius-thickness ratio.
(3) obtain after firing flaky alpha-alumina powder cleaning fused salt after carry out freeze-drying can effectively improve sheet
The dispersibility of alpha-alumina powder.
Detailed description of the invention
Fig. 1 is a kind of preparation flow figure of polymolecularity flaky alpha-alumina powder；
Fig. 2 is the electron scanning micrograph of gained flaky alpha-alumina in the embodiment of the present invention, wherein figure (1),
(2), (3), (4) respectively represent the product of embodiment 1,2,3,4；
Fig. 3 is the XRD spectrum of gained flaky alpha-alumina in the embodiment of the present invention, wherein lines (1), (2), (3), (4)
Respectively represent the product of embodiment 1,2,3,4.
Specific embodiment
Further detailed description is done to the present invention below with reference to example, embodiments of the present invention are not limited thereto.
The present invention provides a kind of polymolecularity flaky alpha-alumina raw powder's production technology, include the following steps: by dissolved with
The Na that 0.03mol -0.09mol carbonate and mass fraction are 0.5% -4%3PO4(relative to the available Al that converts2O3Matter
Measure) the ratio between amount containing 0.01mol-0.03mol aluminium element, fused salt and aluminium element substance is added to as 2:1-with certain rate
The chemical additives that 5:1 and mass fraction are 0.5% -4% are (relative to the available Al that converts2O3Quality) suspension in,
Magnetic stirring apparatus is uniformly mixed with 200r/min -350r/min stirring 30min -40min, is forged after drying with 900 DEG C -1200 DEG C
It burns, 2h -10h is freeze-dried after cleaning fused salt with deionized water to get flaky alpha-alumina uniform, polymolecularity to shape.
Flaky alpha-alumina pattern is observed using scanning electron microscope (SEM).
Following examples, embodiment agents useful for same such as table 1 are carried out according to the method described above.
1 reagent inventory of table
Embodiment 1
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4It is all the 1%SiO that 0.01mol, mass fraction are2
(relative to the available 0.005mol Al that converts2O3Quality, i.e. SiO2Additional amount be 0.0051g, similarly hereinafter) be dissolved in 30ml
Suspension a is made in ionized water；
(2) Na for being 1% by 0.03mol sodium bicarbonate and mass fraction3PO4(relative to the available Al that converts2O3Matter
Amount, similarly hereinafter) it is dissolved in obtained solution b in 30ml deionized water；
(3) solution b is added in suspension a with the rate of sodium bicarbonate 0.01mol/min therein, in magnetic agitation
30min is turned with the revolving speed of 300r/min on device, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1100 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 5h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 16
μm or so, with a thickness of 350nm or so, radius-thickness ratio is 45 or so.
Embodiment 2
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4It is all the 1%SiO that 0.01mol, mass fraction are2
It is dissolved in 30ml deionized water and suspension a is made；
(2) Na for being 1% by 0.015mol sodium carbonate and mass fraction3PO4It is dissolved in obtained solution b in 30ml deionized water；
(3) solution b is added in suspension a with the rate of sodium carbonate 0.01mol/min therein, in magnetic stirring apparatus
On 30min turned with the revolving speed of 300r/min, after dried in electric heating constant-temperature blowing drying box with 65 DEG C；
(4) gel mixture of drying is sintered in Muffle furnace with 1000 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 4h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 14
Microns, with a thickness of 400nm or so, radius-thickness ratio is 35 or so.Embodiment 3
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4It is all the 1%SiO that 0.01mol, mass fraction are2
It is dissolved in 30ml deionized water and suspension a is made；
(2) Na for being 1% by 0.03mol sodium bicarbonate and mass fraction3PO4It is dissolved in obtained solution in 30ml deionized water
b；
(3) solution b is added in suspension a with the rate of the rate 0.005mol/min of sodium bicarbonate therein,
30min is turned with the revolving speed of 300r/min on magnetic stirring apparatus, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1100 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 5h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 13
μm or so, for thickness in 300nm or so, radius-thickness ratio is 43 or so.
Embodiment 4
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4It is all the 1%SiO that 0.01mol, mass fraction are2
It is dissolved in 30ml deionized water and suspension a is made；
(2) Na for being 1% by 0.03mol sodium bicarbonate and mass fraction3PO4It is dissolved in obtained solution in 30ml deionized water
b；
(3) rate by solution b with the rate of sodium bicarbonate therein for 0.0005mol/min is added in suspension a,
30min is turned with the revolving speed of 300r/min on magnetic stirring apparatus, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1000 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 4h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is in 2 μ
M or so, thickness 150nm or so, radius-thickness ratio are 13 or so.
Embodiment 5
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.01mol
Suspension a is made；
(2) 0.03mol sodium bicarbonate is dissolved in obtained solution b in 30ml deionized water；
(3) rate by solution b with the rate of sodium bicarbonate for 0.005mol/min is added in suspension a, in magnetic force
30min is turned with the revolving speed of 300r/min on blender, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1000 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 4h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is in 5 μ
M or so, thickness 200nm or so, radius-thickness ratio are 25 or so.
Embodiment 6
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.015mol
Suspension a is made；
(2) 0.03mol sodium bicarbonate is dissolved in obtained solution b in 30ml deionized water；
(3) rate that the rate of the sodium bicarbonate in solution b is 0.005mol/min is added in suspension a, in magnetic
30min is turned with the revolving speed of 300r/min on power blender, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1000 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 4h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is in 8 μ
M or so, thickness 300nm or so, radius-thickness ratio are 26 or so.
Embodiment 7
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.02mol
Suspension a is made；
(2) 0.03mol sodium bicarbonate is dissolved in obtained solution b in 30ml deionized water；
(3) rate that the rate of the sodium bicarbonate in solution b is 0.005mol/min is added in suspension a, in magnetic
30min is turned with the revolving speed of 300r/min on power blender, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1000 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 4h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is in 8 μ
M or so, thickness 350nm or so, radius-thickness ratio are 22 or so.
Embodiment 8
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.01mol
Suspension a is made；
(2) Na for being 1% by 0.03mol sodium bicarbonate and mass fraction3PO4It is dissolved in obtained solution in 30ml deionized water
b；
(3) sodium bicarbonate in solution b is added in suspension a with the rate of 0.01mol/min, in magnetic stirring apparatus
On 30min turned with the revolving speed of 300r/min, after dried in electric heating constant-temperature blowing drying box with 65 DEG C；
(4) gel mixture of drying is sintered in Muffle furnace with 1100 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 5h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 12
μm or so, with a thickness of 300nm or so, radius-thickness ratio is 40 or so.
Embodiment 9
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.01mol
Suspension a is made；
(2) Na for being 2% by 0.03mol sodium bicarbonate and mass fraction3PO4It is dissolved in obtained solution in 30ml deionized water
b；
(3) solution b is added in suspension a with the rate of sodium bicarbonate 0.01mol/min therein, in magnetic agitation
30min is turned with the revolving speed of 300r/min on device, after in electric heating constant-temperature blowing drying box with 65 DEG C dry；
(4) gel mixture of drying is sintered in Muffle furnace with 1100 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 5h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 11
μm or so, with a thickness of 350nm or so, radius-thickness ratio is 31 or so.
Embodiment 10
(1) by the aluminum sulfate octadecahydrate of 0.005mol, Na2SO4–K2SO4All it is dissolved in 30ml deionized water for 0.01mol
Suspension a is made；
(2) Na for being 4% by 0.03mol sodium bicarbonate and mass fraction3PO4It is dissolved in obtained solution in 30ml deionized water
b；
(3) sodium bicarbonate in solution b is added in suspension a with the rate of 0.01mol/min, in magnetic stirring apparatus
On 30min turned with the revolving speed of 300r/min, after dried in electric heating constant-temperature blowing drying box with 65 DEG C；
(4) gel mixture of drying is sintered in Muffle furnace with 1100 DEG C, keeps the temperature 4h, uses deionization after sintering
Water cleans fused salt, then 5h is lyophilized at -80 DEG C with lyophilized preparation, flaky alpha-alumina is made.Flaky alpha-alumina partial size is 10
μm or so, with a thickness of 400nm or so, radius-thickness ratio is 25 or so.
It is all fine that flaky alpha-alumina dispersibility is obtained by freeze-drying.Solution b is added to the rate in solution a to sheet
The pattern of Alpha-alumina is affected, and the faster embodiment of rate, such as embodiment 1,2, gained flaky alpha-alumina hexagonal is intact
And radius-thickness ratio is big.The amount of addition fused salt also has an impact to the pattern of flaky alpha-alumina, and fused salt has good solvability simultaneously
Promote the growth of crystal, fused salt appropriate can increase the radius-thickness ratio of flaky alpha-alumina, and fused salt can excessively make flaky alpha-alumina
Radius-thickness ratio reduce.Addition sodium phosphate can promote flaky alpha-alumina to form thin slice, can make piece after adding excessive sodium phosphate
The thickness of shape Alpha-alumina increases.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It is equivalent substitute mode, is included within the scope of the present invention.
Claims (9)
1. a kind of polymolecularity flaky alpha-alumina raw powder's production technology, which is characterized in that include the following steps:
(1) deionized water is added to stir and evenly mix silicon source, fused salt, chemical additives to obtain suspension a；
(2) deionized water is added to be uniformly mixed carbonate, dispersing agent to obtain solution b；
(3) the solution b of mixing is added in suspension a, stirs and evenly mixs drying；
(4) gel mixture of drying is calcined, freeze-drying obtains polymolecularity sheet α-after being cleaned with deionized water
Aluminium oxide.
2. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
Suddenly silicon source described in (1) includes aluminum sulfate octadecahydrate, aluminium chloride；The chemical additives include SiO2、TiO2、MnO2,ZnO；
The carbonate includes sodium carbonate, sodium bicarbonate, potassium carbonate, saleratus；The dispersing agent includes Na3PO4。
3. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: outstanding
The ratio between the amount of the substance of aluminium element and the amount of substance of fused salt are 1:(2~5 in turbid a silicon source)；The quality of chemical additives is
It converts available Al relative to by silicon source2O3Quality 0.5% -4%；The amount of the deionized water of addition allows silicon source complete
Fully dissolved.
4. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: molten
The amount of added carbonate makes it carry out completely double hydrolysis or excess with aluminium salt in liquid b；The amount of added dispersing agent is phase
For being converted available Al by silicon source2O3Quality 0.5% -4%.
5. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
Suddenly the stirring rate in (1) and step (2) is 200r/min -350r/min, and mixing time is 30min -40min.
6. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
It is added to solution b in suspension a in 4~360s with average rate in (3) suddenly.
7. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
Suddenly drying temperature described in (3) is 60 DEG C -80 DEG C.
8. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
Suddenly calcination temperature described in (4) is 900 DEG C -1200 DEG C, and the time that calcination temperature is risen to from room temperature is 200min -400min, is forged
Burning soaking time is 4h -6h.
9. a kind of polymolecularity flaky alpha-alumina raw powder's production technology according to claim 1, it is characterised in that: step
Suddenly deionized water wash number described in (4) is 3-4 times, and the freeze-drying temperature is-70 DEG C-- 80 DEG C, sublimation drying
For 2-10h.
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| CN110218995A (en) * | 2019-06-20 | 2019-09-10 | 深圳市绚图新材科技有限公司 | A kind of preparation method of sheet silver packet corundum composite conductive powder |
| CN112978775A (en) * | 2021-04-19 | 2021-06-18 | 陕西科技大学 | Method for preparing flake alumina with high aspect ratio by taking lotus roots as template |
| CN117326579A (en) * | 2023-11-29 | 2024-01-02 | 化学与精细化工广东省实验室 | Method for preparing monodisperse hexagonal flaky alpha-alumina at ultralow temperature |
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| CN112978775A (en) * | 2021-04-19 | 2021-06-18 | 陕西科技大学 | Method for preparing flake alumina with high aspect ratio by taking lotus roots as template |
| CN117326579A (en) * | 2023-11-29 | 2024-01-02 | 化学与精细化工广东省实验室 | Method for preparing monodisperse hexagonal flaky alpha-alumina at ultralow temperature |
| CN117326579B (en) * | 2023-11-29 | 2024-03-08 | 化学与精细化工广东省实验室 | Method for preparing monodisperse hexagonal flaky alpha-alumina at ultralow temperature |
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