CN110407238A - A kind of method that crystal seed method prepares flaky alpha-alumina crystals - Google Patents
A kind of method that crystal seed method prepares flaky alpha-alumina crystals Download PDFInfo
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- CN110407238A CN110407238A CN201910782082.2A CN201910782082A CN110407238A CN 110407238 A CN110407238 A CN 110407238A CN 201910782082 A CN201910782082 A CN 201910782082A CN 110407238 A CN110407238 A CN 110407238A
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- crystal seed
- alumina crystals
- flaky alpha
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- 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
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to a kind of preparation methods of flaky alpha-alumina crystals, belong to powder diameter and pattern control technology field.The flaky alpha-alumina crystals are to hydrolyze the aluminum precursor solution containing water-soluble flux and zinc, tin, phosphorus precursor solution to obtain gel mixture as raw material, and sheet boehmite is crystal seed, then calcines under given conditions, obtains flaky alpha-alumina crystals.The average grain diameter of the flaky alpha-alumina crystals is greater than 20 um, and thickness is greater than 50 less than 0.5 um, radius-thickness ratio.The advantages of a kind of preparation method of flaky alpha-alumina crystals of the present invention has calcination temperature low, and the time is short, at low cost, strong operability.
Description
Technical field
The invention belongs to powder diameters and pattern control technology field, are specifically related to a kind of system of flaky alpha-alumina crystals
Preparation Method.
Background technique
α-Al2O3It is high with hardness, fusing point is high, oxidation resistance is strong, chemical property is stable, thermal conductivity is high, resistivity height etc.
Excellent properties.In addition, bauxite resource rich reserves and cheap.This makes aluminium oxide possess broad application prospect.Sheet oxygen
Change a kind of aluminium oxide of the aluminium as special appearance, not only has the excellent performance of common aluminium oxide, but also due to special
Two-dimensional sheet structure, surface-active is moderate, and adhesive force is strong, to light have the characteristics that the moderate surface-active of albedo,
Good adhesive force, reflection light ability to having obtained large-scale research and development.In addition, in practical applications, leading to
Cross and change synthesis condition to control the crystal morphology (such as thickness, particle diameter distribution, radius-thickness ratio) of tabular alumina, realize structure with
The design of function.Therefore, aluminium oxide of the tabular alumina as a kind of special appearance, has a wide range of applications.Currently, piece
Shape aluminium oxide has been widely used the every field such as pigment, cosmetics, automobile paint vehicle, refractory material, toughening ceramic.
The preparation method of tabular alumina mainly has molte-salt synthesis, hydro-thermal method (solvent-thermal method), high-temperature sintering process etc..
“Chen H, Wu Q, Yang T, et al. The influence of different titanium sources on
flaky α-Al2O3 prepared by molten salt synthesis[J]. Ceramics International,
2015,41 (9): 12288-12294. " has studied the additive of different Ti contents for tabular alumina using molten-salt growth method
Thickness and other patterns α-Al2O3The influence of growth, although obtaining hexagonal plate aluminium oxide, size is smaller, only 9
Um or so.Model is beautiful, Liu Jianghua, the CN105347377B(application number 201510656878.5 of Liu Guanhua application) describe one kind
It is raw material using aluminium isopropoxide, ammonium acid fluoride or ammonium fluoride make crystal morphology controlling agent, then prepare grain under the high temperature conditions
Diameter is the tabular alumina of 2-20 um, but method higher cost is unfavorable for large-scale industrial production.Xu Jie, Cao Yuliang, Xu Hua
The CN107140666A(application number 201710338047.2 of application) describe a kind of utilization nm boehmite, fluoride-mineralization agent
Through ball mill mixing, tabular alumina is then prepared under the high temperature conditions, but the thickness of the tabular alumina of method acquisition is larger.
It can be seen that the tabular alumina prepared at present is there are pattern unevenness, the problems such as particle size is small, and radius-thickness ratio is small.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, a kind of sheet α-Al for possessing big radius-thickness ratio is provided2O3
The preparation method of micro mist, the process flow is simple, is suitble to industrialization large-scale production.
To achieve the above object, technical scheme is as follows:
1. the preparation of tabular alumina presoma
Step 1: the aluminum precursor solution containing water-soluble flux is mixed with zinc, tin precursor solution to prepare metal precursor solutions；
Step 2: with containing carbonate, phosphate solution titration metal precursor solutions to pH6.5-7.5, and hydrating solution is to make
Standby gel mixture；
Step 3: by 90 DEG C age gelation mixture 12 hours, gel mixture is then dried.
2. the synthesis of boehmite seed
Step 1: reaction, which is added dropwise into strong base solution, in the aluminum precursor solution containing water-soluble aluminum salt obtains mixed liquor I；
Step 2: the ethanol solution containing surfactant is added dropwise into mixed liquor I obtains mixed liquor I I；
High-temperature high-voltage reaction is carried out Step 3: mixed liquor I I is transferred in autoclave；
Wherein, the water-soluble aluminum salt in step 1 is one of aluminium chloride, aluminum sulfate, aluminum nitrate or a variety of, and highly basic is strong oxygen
Change one of sodium, potassium hydroxide or a variety of, the concentration of water-soluble aluminum salt is 0.4-0.6 mol/L, Al3+With OH-Molar ratio
For 1:4-1:5;
Wherein, the type of the surfactant in step 2 is cetyl trimethylammonium bromide (CATB), polyvinylpyrrolidine
One of ketone (PVP), lauryl sodium sulfate (SDS), Aerosol OT (AOT) are a variety of, and concentration is
0.02-0.05 mol/L, it is 40%-60% that the ethanol solution of surfactant, which accounts for the volume in mixed liquor I I,；
Wherein, the reaction temperature in step 3 is 120-180 DEG C, and the reaction time is 9-24 h, is centrifuged, and is washed, dry, is obtained
Boehmite seed.
3. the synthesis of tabular alumina
Step 1: tabular alumina presoma is uniformly mixed with crystal seed, mixture is obtained；
Step 2: mixture is carried out high-temperature process；
Step 3: the agglomerate after high-temperature calcination is cooled to room temperature, make it dissolve, is filtered to remove molten in 20-90 DEG C of water
Agent disperses solution using ethyl alcohol and filters, washs, dry, obtains tabular alumina product.
Wherein, the mixing method in step 1 is ball mill mixing or stir mixing, and the additive amount of crystal seed is precursor material
0.05-0.5 wt%；
Wherein, the reaction temperature in step 2 is 1000-1200 DEG C, and the reaction time is 1-5 hours.
Beneficial effect
1, the method that a kind of crystal seed method of the present invention prepares flaky alpha-alumina crystals, prepared tabular alumina partial size ruler
Very little big, radius-thickness ratio is 50 or more；
2, the method that a kind of crystal seed method of the present invention prepares flaky alpha-alumina crystals, device therefor is simple, failure is easy row
It removes, reduce equipment investment；
3, the method that a kind of crystal seed method of the present invention prepares flaky alpha-alumina crystals, technique and easy to operate can carry out big
Large-scale production；
4, the method that a kind of crystal seed method of the present invention prepares flaky alpha-alumina crystals has reaction temperature lower, when reaction
Between it is shorter, the advantages of strong operability.
Detailed description of the invention
Fig. 1 is the boehmite seed transmission electron microscope picture that embodiment 1 is prepared.
Fig. 2 is the XRD diffracting spectrum for the tabular alumina that embodiment 1 is prepared.
Fig. 3 is the surface sweeping electron microscope for the tabular alumina that embodiment 1 is prepared.
Fig. 4 is the surface sweeping electron microscope for the tabular alumina cross section that embodiment 1 is prepared.
Fig. 5 is the particle size distribution figure for the tabular alumina that embodiment 1 is prepared.
Specific embodiment
Carry out the present invention is described in detail below by specific embodiment:
The boehmite seed and tabular alumina of 1-4 of the embodiment of the present invention are detected by following apparatus and method: X-ray
Powder diffractometer (XRD, D8 FOCUS) analyzes the object phase of boehmite seed and tabular alumina；Flied emission surface sweeping Electronic Speculum (SEM,
FEI QUANTAFEG 250) morphology characterization is carried out to tabular alumina；Transmission electron microscope (TEM, JEM-1400) is to vigorous nurse
Stone crystal seed carries out morphology characterization；Laser particle analyzer (BT-9300H) carries out particle size Lambda characterization to tabular alumina.
Case study on implementation 1
In the deionized water containing 250 mL, 66.643 g aluminum sulfate octadecahydrates, 34.090 g sodium sulphate, 27.878 g are added
Potassium sulfate, 0.72 g white vitriol and 0.065 g stannous sulfate.Uniform mixed solution is obtained by mixing at 65 DEG C.
32.755 g sodium carbonate are dissolved in 30 DEG C of 100 mL deionized waters and 0.536 g, ten phosphate dihydrate sodium prepares aqueous slkali.In
While stirring, lye enters aluminum sulfate mixed liquor to pH7.5 dropwise, obtains gel mixture.Then small in 90 DEG C of agings 24
When, 110 DEG C drying 24 hours, the size of the gel mixture of last mill-drying to less than 5 mm.
1.92 g sodium hydroxides are dissolved in 12 mL deionized waters, under agitation, by 20 mL, 0.6 mol/L
Liquor alumini chloridi be added dropwise in sodium hydroxide solution, then be added 40mL 0.05mol/L CATB-C2H5OH solution, is stirred
It mixes 24 hours, after being then transferred to autoclave, 160 DEG C are reacted 12 hours, are then cooled to room temperature, ethanol washing, mistake
Filter, it is dry, obtain boehmite seed.
10 g tabular alumina presomas and 0.012 g boehmite stir mixing are taken, after mixing is uniform.Then, In
1100 DEG C progress calcination processing 2 hours to obtain flaky alpha-alumina crystals.It is cooled to room temperature to crucible, is dissolved in 80 DEG C of water
Flux is isolated by filtration in flux.Then it is washed with water, ethanol washing, in 60 DEG C of dryings, obtaining has 0.1-0.3 um thick
The transparent sheet-like alpha-alumina crystals of degree and 15-35 um partial size.
Case study on implementation 2
SDS-C in addition to 40mL 0.05mol/L is added2H5Other than OH solution, sheet is prepared in the same manner as example 1
Alpha-alumina crystals.Flaky alpha-alumina crystals obtained have the oxidation of the transparent sheet-like of 0.1-0.3 um thickness and 13-31 um partial size
Aluminium crystal.
Case study on implementation 3
Other than 0.01 g boehmite seed is added, flaky alpha-alumina crystals are prepared in the same manner as example 1.It is made
Flaky alpha-alumina crystals have 0.1-0.25 um thickness and 11-28 um partial size transparent sheet-like alpha-alumina crystals.
Case study on implementation 4
Other than 0.015 g boehmite seed is added, flaky alpha-alumina crystals are prepared in the same manner as example 1.System
The flaky alpha-alumina crystals obtained have the transparent sheet-like alpha-alumina crystals of 0.1-0.3 um thickness and 13-32 um partial size.
Case study on implementation 5
Other than 0.025 g boehmite seed is added, flaky alpha-alumina crystals are prepared in the same manner as example 1.System
The flaky alpha-alumina crystals obtained have the transparent sheet-like alpha-alumina crystals of 0.3-0.5 um thickness and 10-26 um partial size.
Case study on implementation 6
Other than boehmite seed is not added, flaky alpha-alumina crystals are prepared in the same manner as example 1.Piece obtained
Shape alpha-alumina crystals have the transparent sheet-like alpha-alumina crystals of 0.2-0.4 um thickness and 9-24 um partial size.
Claims (7)
1. a kind of method that crystal seed method prepares flaky alpha-alumina crystals, it is characterised in that:
Step (1): the aluminum precursor solution containing water-soluble flux is mixed with zinc, tin precursor solution to prepare metal precursor solutions；
Step (2): it uses containing carbonate, phosphate solution titration metal precursor solutions to pH6.5-7.5, and hydrating solution is to make
Standby gel mixture；
Step (3): by 90 DEG C age gelation mixture 12 hours, gel mixture is then dried；
Step (4): reaction is added dropwise into strong base solution in the aluminum precursor solution containing water-soluble aluminum salt and obtains mixed liquor I；
Step (5): and the ethanol solution containing surfactant is added dropwise into mixed liquor I and obtains mixed liquor I I；
Step (6): mixed liquor I I being transferred in autoclave and carries out high-temperature high-voltage reaction, obtains boehmite；
Step (7): tabular alumina presoma is uniformly mixed with crystal seed, obtains mixture；
Step (8): mixture is subjected to high-temperature calcination processing；
Step (9): the agglomerate after high-temperature calcination is cooled to room temperature, is made it dissolve in water, flux is filtered to remove, uses ethyl alcohol
Dispersion solution simultaneously filters, and washs, dry, obtains tabular alumina product.
2. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly the water-soluble aluminum salt in (4) is one of aluminium chloride, aluminum sulfate, aluminum nitrate or a variety of, and highly basic is sodium hydroxide, hydroxide
One of potassium is a variety of, and the concentration of water-soluble aluminum salt is 0.4-0.6 mol/L, Al3+With OH-Molar ratio be 1:4-1:5.
3. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly the type of the surfactant in (5) be cetyl trimethylammonium bromide (CATB), polyvinylpyrrolidone (PVP),
One of lauryl sodium sulfate (SDS), Aerosol OT (AOT) or a variety of, concentration 0.02-0.05
Mol/L, it is 40%-60% that the ethanol solution of surfactant, which accounts for the volume in mixed liquor I I,.
4. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly reaction temperature is 120-180 DEG C in (6), and the reaction time is 9-24 h.
5. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly the crystal seed in (7) is the boehmite obtained in step (6), and partial size is 0.5-5 um, and the content of the crystal seed is presoma
0.05 wt%-0.5wt% of quality.
6. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly the mixing method in (7) is ball mill mixing or stir mixing.
7. the method that a kind of crystal seed method according to claim 1 prepares flaky alpha-alumina crystals, it is characterised in that: the step
Suddenly the calcination temperature in (8) is 1000-1200 DEG C, and calcination time is 1-5 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113620328A (en) * | 2021-08-17 | 2021-11-09 | 苏瓷纳米技术(苏州)有限公司 | Preparation method of nano alumina seed crystal and preparation method of high-purity alumina nanocrystal |
| CN114409883A (en) * | 2021-12-22 | 2022-04-29 | 长兴化学工业(中国)有限公司 | Aluminate glue modified polyester and preparation method thereof, coating and resin film |
| CN114590827A (en) * | 2022-03-22 | 2022-06-07 | 济南大学 | Method for preparing large-particle-size flaky alumina by using flaky alumina seed crystal |
| CN115057458A (en) * | 2022-07-13 | 2022-09-16 | 中国科学院山西煤炭化学研究所 | Method for preparing nano alumina from coal gangue |
| CN116041984A (en) * | 2022-12-30 | 2023-05-02 | 江苏贝丽得新材料有限公司 | Flake alumina with self-weather-resistant function and preparation method thereof |
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| CN115057458A (en) * | 2022-07-13 | 2022-09-16 | 中国科学院山西煤炭化学研究所 | Method for preparing nano alumina from coal gangue |
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| CN116041984A (en) * | 2022-12-30 | 2023-05-02 | 江苏贝丽得新材料有限公司 | Flake alumina with self-weather-resistant function and preparation method thereof |
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Application publication date: 20191105 |