CN103359764B - Preparation method of sheet-shaped alpha-aluminium oxide - Google Patents
Preparation method of sheet-shaped alpha-aluminium oxide Download PDFInfo
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- CN103359764B CN103359764B CN201310287413.8A CN201310287413A CN103359764B CN 103359764 B CN103359764 B CN 103359764B CN 201310287413 A CN201310287413 A CN 201310287413A CN 103359764 B CN103359764 B CN 103359764B
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Abstract
The invention relates to a preparation method of sheet-shaped alpha-Al2O3. The preparation method is characterized by specifically comprising the following steps of: adding alpha-Al2O3 and amorphous Al2O3 into a ball grinding mill for ball grinding to obtain nanometer Al2O3 powder; mixing Na2SO4 with K2SO4, dissolving obtained mixed salt in deionized water, and adding the nanometer Al2O3 to prepare a sizing agent; carrying out ultrasonic treatment on the obtained sizing agent for 0.5-5 hours, and distilling the obtained sizing agent to obtain a mixed material of the Al2O3, the Na2SO4 and the K2SO4; calcining the mixed material of the Al2O3, the Na2SO4 and the K2SO4, and carrying out furnace cooling to room temperature after calcining; and washing the obtained composition with the deionized water to remove the Na2SO4 and the K2SO4 in the composition and finally filtering and drying to obtain the sheet-shaped alpha-Al2O3. According to the preparation method, the sheet-shaped alpha-Al2O3 is prepared by a fused salt method. The preparation method is simple in process and easy in industrial production. The sheet-shaped alpha-aluminium oxide prepared by the invention can be applied to industries of pearlescent pigment, cosmetics and the like and also can be used as a filler of composite material wild phase, advanced abrasives and high polymer materials.
Description
Technical field
The present invention relates to a kind of preparation method of flaky alpha-alumina, can be applicable to coating, the industry such as makeup, wallpaper, printing, also can be used as matrix material wild phase, the base material of senior abrasive, pearly pigment and the filler of macromolecular material.
Background technology
The constitutional features of tabular alumina is that its particle shape is sexangle sheet, and has less thickness and larger radius-thickness ratio, and each particle has the radius-thickness ratio of at least 10: 1.Therefore it is a kind of powder with two-dimension plane structure.Tabular alumina has excellent intrinsic properties and special constitutional features, and therefore, it has many excellent performances:
(1) compared with other flaky powder, tabular alumina has excellent over-all properties, as high in fusing point, hardness is large, physical strength is high, wear resistance is good, resistance to chemical attack, anti-oxidant and good heat resistance etc.
(2) tabular alumina has less thickness and larger radius-thickness ratio, and can reach nano level at thickness direction, and be micron order in radial direction, therefore, it has the double effects of nanometer and micropowder art concurrently; Surfactivity is moderate, effectively can be combined, not easily reunite again and be convenient to effective dispersion with other active group.
(3) tabular alumina has good sticking power, the ability of significant shielding effect and reflection ray.
(4) flaky alumina is close to transparent, colourless, and has the surface of flat-satin, and the crystal of complete crystallization is regular hexagon.
Flaky alumina application widely, can be applicable to pearly pigment, the industries such as makeup, also can be used as matrix material wild phase, the filler of senior abrasive, macromolecular material.
1) for pearly pigment field
Although the matrix of pearly pigment can use the sheet mica of synthetic, artificial mica synthesis sheet is more difficult, and its cost is high, the pearly pigment non-refractory of preparation, and therefore the sheet mica of synthetic is not used widely in pearly pigment field.
In recent years, people have synthesized the powder such as tabular alumina, silicon-dioxide, and are applied to pearly pigment field.The tabular alumina of synthetic not only has the premium properties of natural mica sheet, and especially self advantage: tabular alumina can control or disappear deimpurity introducing in preparation process; Tabular alumina is colorless state, and has smooth surface; The flaky alumina of synthesis has narrower particle diameter and thickness distribution scope; Good dispersity in water, has good stream shape.Tabular alumina has many outstanding performances just, and sheet mica therefore can be replaced to be used for the preparation of pearly pigment.External existing using the research of tabular alumina as pearly pigment matrix at present, but domestic research is little.
2) for cosmetic field
Tabular alumina stable chemical nature is not easily absorbed by the body, and there is good chemical property, higher glossiness and bright color, tabular alumina has good spreadability and adsorptive power after tested, be easy to stick to skin surface and prevent color make-up from coming off, therefore can be used for cosmetic field as additive.Be not that the tabular alumina of any particle diameter may be used to makeup, makeup propose specific structure to used tabular alumina.Generally speaking, the ideal thickness of the slice, thin piece of tabular alumina is 0.2 ~ 1pm, and particle diameter is 2 ~ 40pm.If the thickness of slice, thin piece is greater than 2pm, the reflecting effect of slice, thin piece is just poor, if thickness is less than 0.01pm, the mechanical property of slice, thin piece is just poor, thus affects the adhesivity of makeup effect and makeup.
3) for toughner
Because tabular alumina has good toughness, therefore a certain amount of tabular alumina can be added in pottery and use as toughner.When the generation of this enhancing behavior is due to crack tip stress and the interaction of thermal expansion anisotropy tension stress, produce caused by tiny crack in crack tip region.It can make crackle deflect along the interface between matrix and flaky crystalline grain, thus consumes the energy impelling crack propagation, produces toughening effect by bridging effect, finally plays the effect improving ceramic fracture toughness.Tabular alumina has successfully been prepared Al as crystal seed by the people such as Yoshizawa under hot pressing condition
2o
3pottery, the breaking tenacity of this pottery is 600MPa, and fracture toughness property is that 7.9MPam throws.Not only can strengthen alumina-ceramic using tabular alumina as toughner and can also be used for other pottery toughness reinforcing.
4) for weighting agent
One of purposes the earliest of tabular alumina is exactly use as weighting agent, and the thermal conductivity of aluminum oxide is much larger compared with organism, and therefore tabular alumina is commonly used for the filler of polymkeric substance to strengthen the thermal conductivity of polymkeric substance.Being added in polymkeric substance by a certain amount of tabular alumina makes it form aluminum oxide network in the polymer, most of heat can successfully spread out of by this network, the particle diameter of tabular alumina is larger, the node of the network formed is fewer, thermal conductivity is better, and therefore preparing electronic component with this polymkeric substance one ceramic composite can improve its work-ing life to a great extent.
5) for refractory materials
Plate-like aluminum oxide do refractory material aggregate with or use together with other refractory materialss time have the following advantages: (1) high refractoriness; (2) the good low creepage type of heat load intensity one; (3) high-density, ventilation property is low; (4) good thermal shock resistance; (5) good wear resistance; (6) good erosion resistance; (7) low heat-shrinkable; (8) high purity, reduces impurity to the impact of system.Plate-like aluminum oxide refractory materials for the increasingly severe cruel Iron And Steel Industry of smelting condition, almost include from blast furnace, hotblast stove, hot metal mixer, fish torpedo ladle to the steel teeming ladle of converter, secondary fine furnace, die casting and continuous casting, tundish and hot stove and process furnace etc. the part of useful alumina refractory.
The method preparing sheet-shaped alpha-alumina particles at present has: (1) hydrothermal method, namely refers to, in the pressurized vessel of sealing, with water (or alcohol) for solvent, under the condition of High Temperature High Pressure, carry out chemical reaction; (2) coating method, namely refers to utilize presoma to be mixed with colloidal sol, is coated to by colloidal sol and has on the body material of smooth surface, drying, stripping, obtain flaky powder material; (3) mechanical process, namely refers to utilize the powder mechanically mixing that mechanical force makes by a certain percentage, and in long time running process, powder is under the collision repeatedly of grinding medium, and experience extrudes repeatedly, cold welding and crushing process, becomes the ultrafine particle of Dispersed precipitate; (4) gel-combustion method: sol-gel wet chemical methods and Self-propagating Sintering Synthetic method organically combine by this method, the metal nitrate (oxygenant as combustion processes) preparing oxide compound, as presoma, forms gel with a kind of organic-fuel (reductive agent as combustion processes).In lower temperature heat treatment process, gel quick ignition and burning rapidly, thus obtain metal oxide ceramic body; (5) molten-salt growth method: it is mixed mutually according to a certain percentage the reactant of required component and, two kind of salt, then at the temperature of the fusing point higher than salt, calcination is carried out, define the flux containing salt component, after cooling, obtain powder body material through washed with de-ionized water removing salinity wherein.Wherein hydrothermal method is long for reaction time, has High Temperature High Pressure step, therefore stronger to the dependency of production unit; The powder machinery intensity of the powder gained that coating method obtains is not high, and particle size distribution is wider, needs stage treatment just can reach the requirement of user; The powder purity that mechanical process obtains is low, and required time is longer, because the effect of mechanical force makes crystalline structure wayward by causing the change of grain pattern and physicochemical property; Gel one combustion method complex technical process, gained powder easily produces reunion, and pattern is wayward.Compared with above-mentioned several method, molten-salt growth method equipment is simple, and its reaction can be carried out at a lower temperature, complete in the short period of time, can also be controlled by the pattern of change to powder of the adding of crystal seed or additive, the processing parameter such as fused salt kind and consumption when preparing flaky powder, thus receive the favor of scholars.
Sheet is prepared in molten-salt growth method.In alumina powder jointed preparation process, conventional Al
2(SO
4)
3with Al (OH)
3alumina precursor is obtained by calcination as raw material.Wherein, when Tai-Ace S 150 prepares alumina precursor as raw material, in calcination, SO is had
2, SO
3discharge Deng toxic gas.When aluminium hydroxide prepares alumina precursor as raw material, although synthesis temperature is lower, technological process is simple, pollution-free, aluminium hydroxide is all be that raw material is prepared to come by sodium aluminate usually, and the present invention directly uses α-Al
2o
3with amorphous Al
2o
3for raw material is that tabular alumina prepared by raw material, not only economize in raw materials, simplify operation, simultaneously without obnoxious flavour, liquid discharge, production safety, can promote the use of preparing in flaky alpha-alumina powder industrial production.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of production technique and simply, easily realizes, and cost is lower, and without obnoxious flavour, liquid discharge, product purity is high, epigranular, shape are regular, the preparation method of the tabular alumina of good stability.
In order to solve the problem, the invention provides a kind of sheet α-Al
2o
3preparation method, it is characterized in that, concrete steps comprise:
Step 1: by α-Al
2o
3with amorphous Al
2o
3mass ratio with 1: 1 ~ 1: 20 joins ball milling in ball mill and obtains nanometer Al
2o
3powder;
Step 2: by Na
2sO
4with K
2sO
4with the mass ratio mixing of 1: 1 ~ 1: 5, the mixing salt of gained is dissolved in deionized water, adds the nanometer Al of step 1 gained
2o
3powder makes slurry, nanometer Al in described slurry
2o
3powder and mixing salt mass ratio be 1: 1 ~ 1: 5;
Step 3: slurry ultrasonication 0.5 ~ 5h step 2 obtained, distills gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4compound;
Step 4: by Al
2o
3, Na
2sO
4and K
2sO
4compound be warming up to 700 ~ 1350 DEG C and calcine, after calcining 1-7h, furnace cooling is to room temperature; The synthetics deionized water of gained is carried out the Na washing to remove in synthetics
2sO
4and K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3.
Preferably, the filtrate of described step 4 being filtered gained carries out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The present invention adopts α-Al
2o
3with amorphous Al
2o
3for raw material, add Na
2sO
4, K
2sO
4as fused salt, obtain the α-Al of sheet through high-temperature calcination
2o
3.
The present invention has the advantage that technique is simple, be easy to suitability for industrialized production.Tabular alumina prepared by the present invention can be applicable to pearly pigment, the industries such as makeup, also can be used as matrix material wild phase, the filler of senior abrasive, macromolecular material.
Accompanying drawing explanation
Fig. 1 is the sheet α-Al of embodiment 1 gained
2o
3x-ray diffraction collection of illustrative plates;
Fig. 2 is the sheet α-Al of embodiment 1 gained
2o
3scanning electron microscope (SEM) photograph;
Fig. 3 is the sheet α-Al of embodiment 2 gained
2o
3scanning electron microscope (SEM) photograph;
Fig. 4 is the sheet α-Al of embodiment 3 gained
2o
3scanning electron microscope (SEM) photograph;
Fig. 5 is the sheet α-Al of embodiment 4 gained
2o
3scanning electron microscope (SEM) photograph;
Fig. 6 is the sheet α-Al of embodiment 5 gained
2o
3scanning electron microscope (SEM) photograph.
Embodiment
For making the present invention become apparent, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
Embodiment 1
Adopt α-Al
2o
3with amorphous Al
2o
3for starting raw material, purity is all more than 99.6%, claims the α-Al of 10g
2o
3put into ball mill, by α-Al
2o
3with amorphous Al
2o
3mass ratio 1: 9 take the amorphous Al of 90g
2o
3join ball milling 30h in ball mill and obtain nanometer Al
2o
3powder; By Na
2sO
4with K
2sO
4be made into mixing salt 200g by the mass ratio mixing of 1: 1, and deionized water mixing salt being dissolved in 1000ml obtains salts solution; By 100g nanometer Al
2o
3powder joins in salts solution and makes slurry, by slurry ultrasonication 2h, is distilled by gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4mixture; Said mixture material is placed in the corundum crucible with lid, is placed in High Temperature Furnaces Heating Apparatus and calcines, be warming up to 1000 DEG C with 10 DEG C/min speed and calcine, calcine 4 hours, then cool to room temperature with the furnace, obtain synthetic product; By the synthetic product rinsed with deionized water after above-mentioned calcining 8 times, remove remaining Na
2sO
4, K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3monocrystalline.The filtrate of filtering gained is carried out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The alumina powder jointed of acquisition is detected with X diffraction analysis instrument; As shown in Figure 1, α-Al is only had in diffracting spectrum
2o
3peak; As shown in Figure 2, by scanning electron microscopic observation, the aluminum oxide median size of this sheet is 1 ~ 2um.
Embodiment 2
Adopt α-Al
2o
3with amorphous Al
2o
3for starting raw material, purity is all more than 99.6%, claims the α-Al of 10g
2o
3put into ball mill, by α-Al
2o
3with amorphous Al
2o
3mass ratio 1: 9 take the amorphous Al of 90g
2o
3join ball milling 30h in ball mill and obtain nanometer Al
2o
3powder.By Na
2sO
4with K
2sO
4mass ratio by 1: 1 is made into mixing salt 200g, and deionized water mixing salt being dissolved in 1000ml obtains salts solution.By 100g nanometer Al
2o
3powder joins in salts solution and makes slurry, by slurry ultrasonication 2h, is distilled by gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4mixture; Said mixture material is placed in the corundum crucible with lid, is placed in High Temperature Furnaces Heating Apparatus and calcines, be warming up to 1100 DEG C with 10 DEG C/min speed and calcine, calcination time 3 hours.Cool to room temperature with the furnace, obtain synthetic product.By 8 rinsings of the synthetic product deionized water after above-mentioned calcining, remove remaining Na
2sO
4, K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3monocrystalline.The filtrate of filtering gained is carried out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The alumina powder jointed of acquisition is detected with X diffraction analysis instrument.α-Al is only had in diffracting spectrum
2o
3peak.As shown in Figure 3, by scanning electron microscopic observation, the aluminum oxide median size of this sheet is 1 ~ 3um.
Embodiment 3
Adopt α-Al
2o
3with amorphous Al
2o
3for starting raw material, purity is all more than 99.6%, claims the α-Al of 10g
2o
3put into ball mill, by α-Al
2o
3with amorphous Al
2o
3mass ratio 1: 9 take the amorphous Al of 90g
2o
3join ball milling 30h in ball mill and obtain nanometer Al
2o
3powder.By Na
2sO
4with K
2sO
4mass ratio by 1: 1 is made into mixing salt 200g, and deionized water mixing salt being dissolved in 1000ml obtains salts solution.By 100g nanometer Al
2o
3powder joins in salts solution and makes slurry, by slurry ultrasonication 2h, is distilled by gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4mixture; Said mixture material is placed in the corundum crucible with lid, is placed in High Temperature Furnaces Heating Apparatus and calcines, be warming up to 1200 degree with 10 DEG C/min speed and calcine, calcination time 2 hours.Cool to room temperature with the furnace, obtain synthetic product.By 8 rinsings of the product deionized water after above-mentioned calcining, remove remaining Na
2sO
4, K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3monocrystalline.The filtrate of filtering gained is carried out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The alumina powder jointed of acquisition is detected with X diffraction analysis instrument.α-Al is only had in diffracting spectrum
2o
3peak.As shown in Figure 4, by scanning electron microscopic observation, the aluminum oxide median size of this sheet is 1 ~ 3um.
Embodiment 4
Adopt α-Al
2o
3with amorphous Al
2o
3for starting raw material, purity is all more than 99.6%, claims the α-Al of 10g
2o
3put into ball mill, by α-Al
2o
3with amorphous Al
2o
3mass ratio 1: 9 take the amorphous Al of 90g
2o
3join ball milling 50h in ball mill and obtain nanometer Al
2o
3powder.By Na
2sO
4with K
2sO
4mass ratio by 2: 1 is made into mixing salt 200g, and deionized water mixing salt being dissolved in 1000ml obtains salts solution.By 100g nanometer Al
2o
3powder joins in salts solution and makes slurry, by slurry ultrasonication 2h, is distilled by gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4mixture; Be placed on by said mixture material in the corundum crucible with lid, be placed in High Temperature Furnaces Heating Apparatus and calcine, 10 DEG C/min speed is warming up to 1100 DEG C and calcines, calcination time 3 hours.Cool to room temperature with the furnace, obtain synthetic product.By 8 rinsings of the product deionized water after above-mentioned calcining, remove remaining Na
2sO
4, K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3monocrystalline.The filtrate of filtering gained is carried out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The alumina powder jointed of acquisition is detected with X diffraction analysis instrument.α-Al is only had in diffracting spectrum
2o
3peak.As shown in Figure 5, by scanning electron microscopic observation, the aluminum oxide median size of this sheet is 1 ~ 3um.
Embodiment 5
Adopt α-Al
2o
3with amorphous Al
2o
3for starting raw material, purity is all more than 99.6%, claims the α-Al of 10g
2o
3put into ball mill, by α-Al
2o
3with amorphous Al
2o
3mass ratio 1: 9 take the amorphous Al of 90g
2o
3join ball milling 50h in ball mill and obtain nanometer Al
2o
3powder.By Na
2sO
4with K
2sO
4mass ratio by 3: 1 is made into mixing salt 200g, and deionized water mixing salt being dissolved in 1000ml obtains salts solution.By 100g nanometer Al
2o
3powder joins in salts solution and makes slurry, by slurry ultrasonication 2h, is distilled by gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4mixture; Be placed on by said mixture material in the corundum crucible with lid, be placed in High Temperature Furnaces Heating Apparatus and calcine, 10 DEG C/min speed is warming up to 1100 DEG C, calcination time 3 hours.Cool to room temperature with the furnace, obtain synthetic product.By 8 rinsings of the product deionized water after above-mentioned calcining, remove remaining Na
2sO
4, K
2sO
4, finally by obtaining sheet α-Al after filtration drying
2o
3monocrystalline.The filtrate of filtering gained is carried out Distillation recovery Na
2sO
4and K
2sO
4recycle.
The alumina powder jointed of acquisition is detected with X diffraction analysis instrument.α-Al is only had in diffracting spectrum
2o
3peak.As shown in Figure 6, by scanning electron microscopic observation, the aluminum oxide median size of this sheet is 1 ~ 2um.
Flaky alumina application of the present invention widely, can be applicable to pearly pigment, the industries such as makeup, also can be used as matrix material wild phase, the filler etc. of senior abrasive, macromolecular material.
Claims (1)
1. a sheet α-Al
2o
3preparation method, it is characterized in that, concrete steps comprise:
Step 1: by α-Al
2o
3with amorphous Al
2o
3join ball milling in ball mill with the mass ratio of 1:9 and obtain nanometer Al
2o
3powder;
Step 2: by Na
2sO
4with K
2sO
4mix with the mass ratio of 2:1 or 3:1, the mixing salt of gained is dissolved in deionized water, add the nanometer Al of step 1 gained
2o
3powder makes slurry, nanometer Al in described slurry
2o
3powder and mixing salt mass ratio be 1:2;
Step 3: slurry ultrasonication 0.5 ~ 5h step 2 obtained, distills gained slurry, obtains Al
2o
3, Na
2sO
4and K
2sO
4compound;
Step 4: by Al
2o
3, Na
2sO
4and K
2sO
4compound be warming up to 1000 ~ 1200 DEG C and calcine, after calcining 2-4h, furnace cooling is to room temperature; The synthetics deionized water of gained is carried out the Na washing to remove in synthetics
2sO
4and K
2sO
4, finally by obtaining hexagonal sheet α-Al after filtration drying
2o
3.
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CN104402029B (en) * | 2014-11-18 | 2016-03-02 | 湖北工业大学 | A kind of high dispersive α-Al 2o 3the preparation method of nanometer sheet |
CN104986786B (en) * | 2015-07-31 | 2018-02-27 | 华南理工大学 | A kind of controllable sheet α Al of particle size2O3Powder and preparation method thereof |
CN105731509B (en) * | 2016-05-18 | 2018-01-16 | 湖北大学 | A kind of sheet α Al2O3Powder and preparation method thereof |
CN110182834B (en) * | 2019-05-30 | 2021-09-21 | 浙江瑞成新材料股份有限公司 | Method for preparing flaky alpha-alumina and flaky alpha-alumina |
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CN1936114A (en) * | 2006-09-21 | 2007-03-28 | 上海大学 | Method for preparing flake alpha Al2O3 monocrystal grains at low temperature |
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