CN109205648A - A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination - Google Patents
A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination Download PDFInfo
- Publication number
- CN109205648A CN109205648A CN201710552151.1A CN201710552151A CN109205648A CN 109205648 A CN109205648 A CN 109205648A CN 201710552151 A CN201710552151 A CN 201710552151A CN 109205648 A CN109205648 A CN 109205648A
- Authority
- CN
- China
- Prior art keywords
- microwave
- powder
- crystal seed
- alumina powder
- crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/32—Thermal decomposition of sulfates including complex sulfates, e.g. alums
-
- 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
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
-
- 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
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
-
- 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
-
- 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
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of methods for preparing superfine alumina powder using addition crystal seed and microwave calcination, belong to and prepare aluminum oxide technology field with the thermal decomposition method of aluminium compound.The method for preparing superfine alumina powder using addition crystal seed and microwave calcination of the invention, comprising the following steps: by precursor powder and α-Al2O3Crystal seed is uniformly mixed, and obtains mixing；Mixture is put into auxiliary heating and heat-insulating device, it is intracavitary to be then placed in microwave resonance, and microwave heating keeps the temperature 10~50min to 1050~1200 DEG C, cooled to room temperature to get.Method of the invention can both reduce calcination temperature on the basis of traditional handicraft, substantially shorten calcination time, reduce the partial size of powder, improve powder characteristic, reduce energy consumption, improve production efficiency, and pollution-free；Simultaneously compared to the existing technology for carrying out microwave sintering to presoma powder, microwave sintering process is further simplified, energy consumption is reduced and the granularity of powder and reduces reunion.
Description
Technical field
The present invention relates to a kind of methods for preparing superfine alumina powder using addition crystal seed and microwave calcination, belong to and use aluminium
The thermal decomposition method of compound prepares aluminum oxide technology field.
Background technique
China's alumina product is the especially low sodium of ultra-fine alumina, ultra-fine, high purity aluminium oxide based on commercial alumina
Industrialization level has not yet been reached in production, and product relies primarily on import.It is high-grade with the continuous development of domestic new high-tech industry
Secondary, multiform alumina demand is continuously increased.High purity aluminium oxide refers to that purity is greater than 99.99%, even-grained Ultramicro-powder
Body material is most wide one of the tip materials of 21 century yield maximum, output value highest, purposes.High-purity ultra-fine alumina has height
Hardness, high intensity, wear-resistant, corrosion-resistant, high temperature resistant, anti-oxidant, good insulating, surface area is big, thermal expansion coefficient is small, anti-thermal shock
The excellent characteristics such as performance is good, dielectric loss is low are widely used in insulating materials, electronic product, abrasion-proof corrosion-proof corrosion material and boat
The high-tech such as empty space material tip industry.In recent years, high purity aluminium oxide ink-jet printer paper and coating, display material,
The energy, automobile, semiconductor and PC domain obtain expanding application, especially whole world LED fast development and national illuminating engineering
Implementation, demand increases sharply, and yield increases rapidly.Therefore, high purity aluminium oxide has broad application prospects.
The preparation method of high purity aluminium oxide is varied, is broadly divided into solid phase method, liquid phase method and vapor phase method three categories.It is common
Specific method have hydrothermal synthesis method, sol-gal process, improvement Bayer process, organo-aluminium alkoxide hydrolysis, spark discharge method etc.,
Wherein hydrothermal synthesis method can prepare the high purity aluminium oxide of favorable dispersibility, but its technique need to carry out at high temperature, be produced into
This is higher, and can generate explosive gas hydrogen, and there are security risks；Sol-gal process simple process, but product is easy
Existing hard aggregation phenomenon；It is extensive to improve Bayer process raw material, it is at low cost, but sodium oxide content is high in product, limited purity；Organic alfol
Salt water solution can prepare the thinner ultra micro aluminium oxide of primary particle, but its product is reunited seriously, and production cost is higher；Electric spark
Electric discharge is able to achieve clean manufacturing, but there are major safety risks in production process, consume energy larger.Therefore, it is a kind of low cost, can
Repeatability technology that is strong, pollution-free, can be mass high purity alumina powder is urgently researched and developed.It can be realized industrialized production at present
Method have three kinds of aluminium isopropoxide Hydrolyze method, alum pyrolysismethod and aluminium carbonate ammonium pyrolysismethod, wherein alum pyrolysismethod
Raw material sources are extensive, simple production process, can prepare 5N grades of high purity aluminium oxides, but its calcination temperature is higher, easily makes product
Reunite, and it is higher to consume energy.
Microwave is a kind of electromagnetic wave between radio wave and infrared ray wave band, wave-length coverage 1mm~1m, frequency model
It encloses for 300MHz~300GHz, since frequency is very high, so also referred to as uhf electromagnetic wave.Microwave heating refers to compound in electricity
It is heated in vivo as caused by dielectric loss in magnetic field, microwave heating is to absorb microwave energy by object to be translated into thermal energy,
Keep itself whole while heating heating method.Microwave heating technique is transported by heated object internal dipole molecule high-frequency reciprocating
Movable property raw " interior frictional heat " and increase heating object temperature, be not necessarily to any heat transfer process, object is inside and outside to heat liter simultaneously
Temperature, heating speed are fast and uniformly, it is only necessary to which the part of traditional heating mode 1/tens can reach heating purpose.
Compared with traditional heating mode, microwave heating is fast with heating rate, homogeneous heating, controllability are strong, selectivity heating, reacts spirit
Quick, penetration power is strong, cleaning, it is pollution-free the advantages that.
In the prior art, Authorization Notice No. is that CN102531014B Chinese invention patent discloses a kind of α-Al2O3Powder
Hybrid microwave sintering process is to be placed in presoma powder in auxiliary heating and heat-insulating device, assists heating and heat-insulating device and presoma
Powder is put into that microwave resonance is intracavitary to be sintered together: firstly, opening microwave source, microwave input power is adjusted, with average 6~30
DEG C/speed of min slowly heats up；After to be drained off, start to continuously adjust microwave input power, with 20~100 DEG C/min's
Speed heats rapidly, while monitoring reflection power；When power stability to be reflected, maintain heating rate 10~30 DEG C/min at the uniform velocity
1000~1500 DEG C of sintering temperature are warming up to, 2~20min is kept the temperature, control microwave input power is even with the speed of 6~30 DEG C/min
Speed is cooled to room temperature to get α-Al2O3Powder body；Wherein, auxiliary heating and heat-insulating device includes the inside and outside double-deck insulating layer, interior
It is equipped with auxiliary heating body between outer double insulation, is provided at the top of inside and outside double insulation and the matched cover board of its shape, lid
Infrared measurement of temperature hole is offered on plate.Although this method can be realized crystal grain refinement and homogenization, reduce hard group to a certain extent
It is poly-, but the α-Al of this method preparation2O3Powder average grain diameter is larger, and is also required to carry out microwave heating control in cooling procedure
Rate of temperature fall, entire sintering process is complex, and energy consumption is high, the unfavorable popularization and application with industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of simple process, energy-efficient utilization addition crystal seed and microwave calcinations to prepare ultra-fine oxygen
Change the method for aluminium powder body.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A method of using addition crystal seed and microwave calcination prepare superfine alumina powder, comprising the following steps: will before
Drive body powder and α-Al2O3Crystal seed is uniformly mixed, and obtains mixing；Mixing is put into auxiliary heating and heat-insulating device, then auxiliary is heated
It is intracavitary that attemperator is put into microwave resonance, and microwave heating keeps the temperature 10~50min, at room temperature natural cooling to 1050~1200 DEG C,
To obtain the final product.
The method for preparing superfine alumina powder using addition crystal seed and microwave calcination of the invention, by precursor
α-Al is added in material2O3Crystal seed is directly cooled down after calcining, can be prepared by granularity between 100~200nm, favorable dispersibility
α-Al2O3Powder.Method of the invention both can reduce calcination temperature on the basis of traditional handicraft, be greatly shortened and forge
The time is burnt, the partial size of powder is reduced, improves powder characteristic, reduce energy consumption, improve production efficiency, and pollution-free；
Simultaneously compared to the existing technology for carrying out microwave sintering to presoma powder, further simplifies the technique of microwave sintering, reduces
Energy consumption and the granularity of powder simultaneously reduce reunion, meet the development strategy of China's " circular economy ", have good Environmental Effect
Benefit, economic benefit and social benefit.
α-Al in the mixing2O3The mass percent of crystal seed is 0.1~0.85%.
In mixing, α-Al2O3The partial size of crystal seed is 100~200nm.
In mixing, the partial size of presoma powder is 3~10 μm.
Before heat preservation, the heating rate of microwave heating is 15~25 DEG C/min.Insulating process carries out under microwave continuous heating.
The auxiliary heating and heat-insulating device includes the chamber for being used to accommodate the mixing that insulating layer and insulating layer surround
Body；The insulating layer includes outer heat insulation layer and the inside holding microwave absorbing material coating that outer heat insulation layer inner wall is arranged in.
Preferably, the outer heat insulation layer includes the tubular outer heat insulation layer ontology of both ends open, and respectively with both ends open
Seal the outer heat insulation layer first end cover and outer heat insulation layer second end cover of cooperation；The tubular outer heat insulation layer ontology and outer heat insulation layer the
The cavity is formed after one end cap and the sealing cooperation of outer heat insulation layer second end cover.The inside holding absorbing material coating is arranged in institute
State the inner wall of tubular outer heat insulation layer ontology.The outer heat insulation layer first end cover is equipped with for penetrating in the cavity for thermocouple
Thermometer hole.
Absorbing material in the inside holding absorbing material coating is SiC.The outer heat insulation layer is made of mullite.
By mixing be put into microwave resonance it is intracavitary when, be first by mixing be put into auxiliary heating and heat-insulating device in, be then placed in micro-
In wave resonance chamber.During alumina transition opposite α inversion of phases, cold stage aluminium oxide absorbing property is poor, interior at this time
Thermal-insulation microwave absorbing material coating can absorb microwave, plays the role of auxiliary heating, and after reaching critical-temperature, aluminium oxide itself is inhaled
Wave heating is to sintering temperature.
The presoma powder is Monoaluminum monoammonium disulfate Dodecahydrate.
High purity aluminium oxide in order to obtain, the purity of used Monoaluminum monoammonium disulfate Dodecahydrate are 4N~5N grades.It is pure using this
The Monoaluminum monoammonium disulfate Dodecahydrate for spending rank, can prepare α-Al of the purity 99.995% or more2O3Powder.The rank purity
Monoaluminum monoammonium disulfate Dodecahydrate can be prepared using method comprising the following steps:
1) saturated solution of the two of the aluminum sulfate containing the amount for waiting substances and ammonium sulfate is mixed, is steamed at 60~80 DEG C
It has been sent to crystalline membrane appearance, ethyl alcohol is then added, 0~10 DEG C is cooled under stirring, has been stood, until crystal is precipitated completely；
2) crystal being precipitated in step 1) filtered, washed, dried, obtain alum crystal crude product；
3) alum crystal crude product is dissolved in water, then solution has been evaporated to crystalline membrane at 60~80 DEG C and has been gone out
It is existing, minimal amount of water is added, dissolves crystallization just, the tartaric acid of alum crystal crude product quality 3~5% is then added
Ammonium stirs 10~20min, filters while hot, regathers filtrate；
4) ethyl alcohol is added into filtrate, stirs, is then stood in mixture of ice and water and is cooled to crystal and is precipitated completely；
5) crystal being precipitated in step 4) filtered, washed, dried, obtain the alum recrystallized for the first time；
6) repeat step 3)~5) carry out repeated recrystallize to get.
In step 1) and step 4), it is the 10~60% of liquor capacity that ethyl alcohol volume, which is added,.The ethyl alcohol is anhydrous second
Alcohol.After dehydrated alcohol is added, the speed of crystallization is accelerated, while crystallization amount also greatly increases.
In step 1) and step 5), the stirring is to be vigorously stirred.In step 5), the time of the stirring is 5min.
In step 2) and step 5), the drying can be dried by the way of microwave heating；When dry, microwave adds
Heat is to 50~70 DEG C of 5~10min of heat preservation.Heating rate when microwave heating is 25~35 DEG C/min.Using the side of microwave heating
Formula is dried, and is polar molecule using hydrone, microwave is can absorb in microwave field, the evaporation that is rapidly heated may be implemented, add
Fast rate of drying.
In step 2), the washing is using water and ethyl alcohol alternately 3~5 times washings.
In step 3), solution can also be evaporated to crystal at 60~80 DEG C will be precipitated, and then be filtered while hot again.
In step 3), after ammonium tartrate solution is added into solution, ammonium tartrate can form complex compound with foreign ion.
In step 4), the standing cooling makes the temperature of filtrate be down to 0~5 DEG C.Stand the cooling time be 10~
30min。
Described to be mixed into ball milling, the revolving speed of ball milling is 3000~8000r/min, and the time is 3~8min.Preferably, described
Ball milling is high-energy ball milling.
α-the Al2O3The preparation method of crystal seed, comprising the following steps:
A) it is 8.0~10.0 that ammonium hydroxide is added dropwise in the aluminum salt solution that aluminium ion concentration is 0.6~1.0mol/l to pH, is generated
Al(OH)3Colloid；
B) by Al obtained in step a) (OH)3Colloid settles 1~3h, then the colloid after sedimentation is cleaned, is dried,
It obtains Al (OH)3Gel；
C) by Al (OH)3Gel is calcined at 1100~1300 DEG C, keep the temperature 20~50min to get.
In step a), the aluminum salt solution is aluminum sulfate solution.
In step b), the cleaning is using water and ethyl alcohol alternately cleaning 3~5 times.
In step b), the temperature of the drying is 60~100 DEG C, and the time is 20~28h.
Detailed description of the invention
Fig. 1 is the XRD diagram of the Monoaluminum monoammonium disulfate Dodecahydrate obtained after recrystallizing three times in embodiment 1；
Fig. 2 is ultra-fine α-Al obtained by embodiment 1 and comparative example 21~222O3The XRD diagram of powder；
Fig. 3 is α-Al obtained by comparative example 1~42O3The XRD diagram of powder；
Fig. 4 is α-Al obtained by comparative example 5~92O3The XRD diagram of powder；
Fig. 5 is α-Al obtained by comparative example 10~142O3The XRD diagram of powder；
Fig. 6 is α-Al obtained by comparative example 15~172O3The XRD diagram of powder；
Fig. 7 is α-Al obtained by comparative example 18~202O3The XRD diagram of powder；
Fig. 8 is α-Al made from comparative example 32O3The test picture of powder；Wherein, Fig. 8 a is SEM figure, and Fig. 8 b is granularity point
Butut；
Fig. 9 is α-Al made from comparative example 42O3The test picture of powder；Wherein, Fig. 9 a is SEM figure, and Fig. 9 b is granularity point
Butut；
Figure 10 is α-Al made from comparative example 122O3The test picture of powder；Wherein, Figure 10 a is SEM figure, and Figure 10 b is grain
Spend distribution map；
Figure 11 is α-Al made from comparative example 152O3The test picture of powder；Wherein, Figure 11 a is SEM figure, and Figure 11 b is grain
Spend distribution map；
Figure 12 is α-Al made from embodiment 12O3The test picture of powder；Wherein, Figure 12 a is SEM figure, and Figure 12 b is granularity
Distribution map；
Figure 13 is the structural schematic diagram of auxiliary heating and heat-insulating device used by Examples 1 to 3.
Specific embodiment
Below in conjunction with specific embodiment, further description of the technical solution of the present invention.
α-Al employed in each embodiment2O3Crystal seed is prepared using following methods:
1) compound concentration is the aluminum sulfate solution of 0.8mol/L；
2) ammonium hydroxide is added dropwise after filtering solution, adjusts pH value to 9.0, generates Al (OH)3Colloid；
3) by Al obtained in step 2) (OH)3Colloid settles 2h, then will cleaning using alternately cleaning 4 times of water, ethyl alcohol
Drying for 24 hours, obtains Al (OH) at 80 DEG C of colloid afterwards3Gel；
4) by Al (OH)3Gel is calcined at 1150 DEG C, keep the temperature 30min to get.
Used auxiliary heating and heat-insulating device is as shown in figure 13 when microwave calcination in each embodiment, including insulating layer, with
And the cavity 4 for being used to accommodate mixing that insulating layer surrounds；The insulating layer includes outer heat insulation layer and is arranged in outer heat insulation layer inner wall
SiC coating 6；The outer heat insulation layer includes the tubular outer heat insulation layer ontology 1 of upper and lower ends opening, and is sealed with upper end opening
The outer heat insulation layer first end cover 2 of cooperation, the outer heat insulation layer second end cover 3 with lower ending opening sealing cooperation；Tubular outer heat insulation layer sheet
Body 1 forms the cavity for accommodating mixing with after outer heat insulation layer first end cover 2 and the lid sealing cooperation of outer heat insulation layer second end 3 respectively
4；The external thermal insulation first end cover is equipped with thermometer hole 5, and thermocouple enters in cavity 4 after passing through thermometer hole 5；The SiC coating 6
The inner wall of the tubular outer heat insulation layer ontology 1 is set.In use, mixing is put into outer heat insulation layer ontology and outer heat insulation layer second
In the cavity that end cap cooperatively forms, outer heat insulation layer first end cover is then covered, auxiliary heating and heat-insulating device is put into microwave resonance
It is intracavitary.
Embodiment 1
The method for preparing superfine alumina powder using addition crystal seed and microwave calcination of the present embodiment, including following step
It is rapid:
A precursor powder) is prepared
Precursor powder is prepared using the method included the following steps:
1) by Al2(SO4)3·18H2O is dissolved in distilled water, and stirring is to transparent at 70 DEG C, and by solution filter membrane mistake
Filter keeps filtrate fully transparent；(the NH of equimolar amounts is taken simultaneously4)2SO4It is dissolved in distilled water, filtering keeps transparent；By above-mentioned two
Kind of solution is evaporated to when just crystallizing out, then crystallization is dissolved in the water of minimum flow, is reached saturation, is respectively obtained saturation sulphur
Sour aluminum solutions and saturated ammonium sulfate solution；
2) above two saturated solution is mixed, the heating water bath mixed solution at 70 DEG C has been evaporated to crystalline membrane and has gone out
It is existing, the dehydrated alcohol of mixed liquor volume 30% is then added, then mixed solution is cooled to 5 in the case where being vigorously stirred
DEG C, 20min is stood, until crystal is precipitated completely；
3) it will precipitate crystal and filter on a buchner funnel, and replace cleaning 5 times with distilled water and dehydrated alcohol, then microwave
60 DEG C of (heating rate is 30 DEG C/min) dry 5min are heated to, alum coarse crystallization product is obtained；
4) alum coarse crystallization product is dissolved in distilled water, solution is placed in water-bath after dissolution, under the conditions of 70 DEG C
It has been evaporated to crystalline membrane appearance, then crystallization has been dissolved in minimum flow water；Then alum crude product matter is added into solution
4% ammonium tartrate of amount stirs 15min, then filters while hot, filters off some insoluble matter impurity, collects filtrate；
5) 30% dehydrated alcohol of molten aluminum volume is added into filtrate, is vigorously stirred 5min, is then placed in mixture of ice and water
Middle standing cooling, the temperature for controlling filtrate is 1 DEG C, until crystal is precipitated completely；Then it is filtered, obtained crystal is carried out
Washing, then microwave heating obtains the aluminum sulfate recrystallized for the first time to 60 DEG C of (heating rate is 30 DEG C/min) dry 5min
Ammonium crystal；
6) repeat 3)~5) step, carry out 3 times recrystallize be made Monoaluminum monoammonium disulfate Dodecahydrate crystal to get；
B) microwave calcination
By α-Al2O3Crystal seed and Monoaluminum monoammonium disulfate Dodecahydrate powder obtained are under the revolving speed of 8000r/min, high-energy ball milling
3min obtains mixing；Mixing is put into auxiliary heating and heat-insulating device, auxiliary heating and heat-insulating device is then put into microwave resonance again
It is intracavitary, with the heating rate microwave heating of 20 DEG C/min to 1050 DEG C, keep the temperature 30min, at room temperature natural cooling to get；α-
Al2O3Crystal seed accounts for the 0.582% of mixing gross mass；After high-energy ball milling, α-Al in mixing2O3The partial size of crystal seed be 100nm, 12
The partial size of hydrazine aluminum sulfate ammonium is 5 μm.
Superfine alumina powder made from the present embodiment is α-Al2O3Powder, by α-Al2O3The partial size and ratio of powder
Surface area carries out analysis detection, it is known that the resulting α-Al of the present embodiment2O3The partial size of powder is 105nm, specific surface area 108m2/
g。
In addition, α-Al resulting to the present embodiment2O3Powder carries out constituent analysis, and analysis the results are shown in Table 1.
Resulting α-the Al of 1 embodiment of table 12O3The content of the composition of powder and each ingredient
Embodiment 2
The method for preparing superfine alumina powder using addition crystal seed and microwave calcination of the present embodiment, including following step
It is rapid:
A precursor powder) is prepared
Precursor powder is prepared using the method included the following steps:
1) by Al2(SO4)3·18H2O is dissolved in distilled water, and stirring is to transparent at 60 DEG C, and by solution filter membrane mistake
Filter keeps filtrate fully transparent；(the NH of equimolar amounts is taken simultaneously4)2SO4It is dissolved in distilled water, filtering keeps transparent；By above-mentioned two
Kind of solution is evaporated to when just crystallizing out, then crystallization is dissolved in the water of minimum flow, is reached saturation, is respectively obtained saturation sulphur
Sour aluminum solutions and saturated ammonium sulfate solution；
2) above two saturated solution is mixed, the heating water bath mixed solution at 80 DEG C has been evaporated to crystalline membrane and has gone out
It is existing, the dehydrated alcohol of mixed liquor volume 60% is then added, then mixed solution is cooled to 0 in the case where being vigorously stirred
DEG C, 20min is stood, until crystal is precipitated completely；
3) it will precipitate crystal and filter on a buchner funnel, and replace cleaning 3 times with distilled water and dehydrated alcohol, then microwave
70 DEG C of (heating rate is 25 DEG C/min) dry 7min are heated to, alum coarse crystallization product is obtained；
4) alum coarse crystallization product is dissolved in distilled water, solution is placed in water-bath after dissolution, under the conditions of 60 DEG C
It has been evaporated to crystalline membrane appearance, then crystallization has been dissolved in minimum flow water；Then alum crude product matter is added into solution
5% ammonium tartrate of amount stirs 20min, then filters while hot, filters off some insoluble matter impurity, collects filtrate；
5) 10% dehydrated alcohol of molten aluminum volume is added into filtrate, is vigorously stirred 5min, is then placed in mixture of ice and water
Middle standing cooling, the temperature for controlling filtrate is 0 DEG C, until crystal is precipitated completely；Then it is filtered, obtained crystal is carried out
Washing, then microwave heating obtains the aluminum sulfate recrystallized for the first time to 50 DEG C of (heating rate is 25 DEG C/min) dry 10min
Ammonium crystal；
6) repeat 3)~5) step, carry out 4 times recrystallize be made Monoaluminum monoammonium disulfate Dodecahydrate crystal to get；
B) microwave calcination
By α-Al2O3Crystal seed and Monoaluminum monoammonium disulfate Dodecahydrate powder obtained are under the revolving speed of 5000r/min, high-energy ball milling
5min obtains mixing；Mixing is put into auxiliary heating and heat-insulating device, auxiliary heating and heat-insulating device is then put into microwave resonance again
It is intracavitary, with the heating rate microwave heating of 15 DEG C/min to 1200 DEG C, keep the temperature 10min, at room temperature natural cooling to get；α-
Al2O3Crystal seed accounts for the 0.839% of mixing gross mass；After high-energy ball milling, α-Al in mixing2O3The partial size of crystal seed be 150nm, 12
The partial size of hydrazine aluminum sulfate ammonium is 10 μm.
Superfine alumina powder made from the present embodiment is α-Al2O3Powder, by α-Al2O3The partial size and ratio of powder
Surface area carries out analysis detection, it is known that the resulting α-Al of the present embodiment2O3The partial size of powder is 184nm, specific surface area 14m2/
g。
Embodiment 3
The method for preparing superfine alumina powder using addition crystal seed and microwave calcination of the present embodiment, including following step
It is rapid:
A precursor powder) is prepared
Precursor powder is prepared using the method included the following steps:
1) by Al2(SO4)3·18H2O is dissolved in distilled water, and stirring is to transparent at 80 DEG C, and by solution filter membrane mistake
Filter keeps filtrate fully transparent；(the NH of equimolar amounts is taken simultaneously4)2SO4It is dissolved in distilled water, filtering keeps transparent；By above-mentioned two
Kind of solution is evaporated to when just crystallizing out, then crystallization is dissolved in the water of minimum flow, is reached saturation, is respectively obtained saturation sulphur
Sour aluminum solutions and saturated ammonium sulfate solution；
2) above two saturated solution is mixed, the heating water bath mixed solution at 60 DEG C has been evaporated to crystalline membrane and has gone out
It is existing, the dehydrated alcohol of mixed liquor volume 10% is then added, then mixed solution is cooled to 10 in the case where being vigorously stirred
DEG C, 20min is stood, until crystal is precipitated completely；
3) it will precipitate crystal and filter on a buchner funnel, and replace cleaning 4 times with distilled water and dehydrated alcohol, then microwave
50 DEG C of (heating rate is 35 DEG C/min) dry 10min are heated to, alum coarse crystallization product is obtained；
4) alum coarse crystallization product is dissolved in distilled water, solution is placed in water-bath after dissolution, under the conditions of 80 DEG C
It has been evaporated to crystalline membrane appearance, then crystallization has been dissolved in minimum flow water；Then alum crude product matter is added into solution
3% ammonium tartrate of amount stirs 10min, then filters while hot, filters off some insoluble matter impurity, collects filtrate；
5) 60% dehydrated alcohol of molten aluminum volume is added into filtrate, is vigorously stirred 5min, is then placed in mixture of ice and water
Middle standing cooling, the temperature for controlling filtrate is 5 DEG C, until crystal is precipitated completely；Then it is filtered, obtained crystal is carried out
Washing, then microwave heating obtains the aluminum sulfate recrystallized for the first time to 70 DEG C of (heating rate is 35 DEG C/min) dry 6min
Ammonium crystal；
6) repeat 3)~5) step, carry out 5 times recrystallize be made Monoaluminum monoammonium disulfate Dodecahydrate crystal to get；
B) microwave calcination
By α-Al2O3Crystal seed and Monoaluminum monoammonium disulfate Dodecahydrate powder obtained are under the revolving speed of 3000r/min, high-energy ball milling
8min obtains mixing；Mixing is put into auxiliary heating and heat-insulating device, auxiliary heating and heat-insulating device is then put into microwave resonance again
It is intracavitary, with the heating rate microwave heating of 25 DEG C/min to 1120 DEG C, keep the temperature 50min, at room temperature natural cooling to get；α-
Al2O3Crystal seed accounts for the 0.113% of mixing gross mass；After high-energy ball milling, α-Al in mixing2O3The partial size of crystal seed be 200nm, 12
The partial size of hydrazine aluminum sulfate ammonium is 3 μm.
Superfine alumina powder made from the present embodiment is α-Al2O3Powder, by α-Al2O3The partial size and ratio of powder
Surface area carries out analysis detection, it is known that the resulting α-Al of the present embodiment2O3The partial size of powder is 142nm, specific surface area 53m2/
g。
Comparative example 1
The alumina powder of this comparative example is using the method preparation included the following steps: Monoaluminum monoammonium disulfate Dodecahydrate is put into
In Muffle furnace, Muffle furnace is raised to 250 DEG C from room temperature, heating rate is 2 DEG C/min；Then with the rate of 5 DEG C/min after of continuing rising
Temperature keeps the temperature 30min to 550 DEG C；Then 900 DEG C are warming up to the rate of 5 DEG C/min, keep the temperature 2h；Finally with the speed of 5 DEG C/min
Rate is warming up to Tm, keep the temperature 2h to get；Wherein, Tm=1300 DEG C.
Comparative example 2
The preparation method of the alumina powder of this comparative example removes Tm=1200 DEG C outer, remaining is completely the same as comparative example 1.
Comparative example 3
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 1.
Comparative example 4
The preparation method of the alumina powder of this comparative example removes Tm=1000 DEG C outer, remaining is completely the same as comparative example 1.
Comparative example 5
The alumina powder of this comparative example is using the method preparation included the following steps:
Mixing obtained in embodiment 3 is put into Muffle furnace, Muffle furnace is raised to 250 DEG C from room temperature, heating rate 2
℃/min；Then continue to be warming up to 550 DEG C with the rate of 5 DEG C/min, and keep the temperature 30min；Then it is heated up with the rate of 5 DEG C/min
To 900 DEG C, 2h is kept the temperature；T is finally warming up to the rate of 5 DEG C/minm, keep the temperature 2h to get；Wherein, Tm=1050 DEG C.
Comparative example 6
The preparation method of the alumina powder of this comparative example, by α-Al2O3Crystal seed and Monoaluminum monoammonium disulfate Dodecahydrate powder exist
Under the revolving speed of 8000r/min, high-energy ball milling 3min obtains mixing；α-Al in mixing2O3Powder accounts for the 0.347% of mixing gross mass；
α-Al in mixing2O3Partial size be 200nm, the partial size of Monoaluminum monoammonium disulfate Dodecahydrate is 3 μm, remaining is completely the same as comparative example 5.
Comparative example 7
The preparation method of the alumina powder of this comparative example is prepared except the mixing used for the method for embodiment 1
Remaining is completely the same as comparative example 5 outside mixing.
Comparative example 8
The preparation method of the alumina powder of this comparative example is prepared except the mixing used for the method for embodiment 2
Outside mixing, remaining is completely the same as comparative example 5.
Comparative example 9
The preparation method of the alumina powder of this comparative example, in addition to the powder of calcining is to be not added with the presoma of crystal seed,
It is remaining completely with comparative example 5.
Comparative example 10
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 5.
Comparative example 11
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 6.
Comparative example 12
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 7.
Comparative example 13
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 8.
Comparative example 14
The preparation method of the alumina powder of this comparative example removes Tm=1100 DEG C outer, remaining is completely the same as comparative example 1.
Comparative example 15
The method that the microwave calcination of this comparative example prepares alumina powder, comprising the following steps: weigh a certain amount of 12
Water ammonium aluminum sulfate crystal is put into corundum crucible, is heated to 1100 under microwave heating system with the heating rate of 15 DEG C/min
DEG C, 10min is kept the temperature, natural cooling, obtains product at room temperature.
Comparative example 16
The method that the microwave calcination of this comparative example prepares alumina powder, comprising the following steps: weigh a certain amount of 12
Water ammonium aluminum sulfate crystal is put into corundum crucible, is heated to 1100 under microwave heating system with the heating rate of 20 DEG C/min
DEG C, 30min is kept the temperature, natural cooling, obtains product at room temperature.
Comparative example 17
The method that the microwave calcination of this comparative example prepares alumina powder, comprising the following steps: weigh a certain amount of 12
Water ammonium aluminum sulfate crystal is put into corundum crucible, is heated to 1100 under microwave heating system with the heating rate of 25 DEG C/min
DEG C, 50min is kept the temperature, natural cooling, obtains product at room temperature.
Comparative example 18
The method that the microwave calcination of this comparative example prepares alumina powder, except being by presoma powder microwave heating to 1150
Outside DEG C being kept the temperature, remaining is completely the same as embodiment 16.
Comparative example 19
The method that the microwave calcination of this comparative example prepares alumina powder, except being by presoma powder microwave heating to 1150
Outside DEG C being kept the temperature, remaining is completely the same as embodiment 17.
Comparative example 20
The method that the microwave calcination of this comparative example prepares alumina powder, except being by presoma powder microwave heating to 1150
Outside DEG C being kept the temperature, remaining is completely the same as embodiment 18.
Comparative example 21
The preparation method of the alumina powder of this comparative example, except the heating rate before microwave heating is 20 DEG C/min, microwave
The temperature of heating is 1000 DEG C, soaking time is outside 30min, remaining is completely the same as embodiment 2.
Comparative example 22
The preparation method of the alumina powder of this comparative example, except the heating rate before microwave heating is 20 DEG C/min, microwave
The temperature of heating is 950 DEG C, soaking time is outside 30min, remaining is completely the same as embodiment 3.
Experimental example 1
Respectively to α-Al obtained by embodiment 1 and comparative example 1~222O3Powder carries out XRD test, test result difference
See Fig. 2~7.
As shown in Figure 2, α-Al is added using microwave calcination as seen from the figure2O3When the precursor powder of crystal seed, at 1050 DEG C
Good α-the Al of crystallinity can be prepared2O3Powder is unable to get α phase lower than this temperature.
It is only α-in 1200 DEG C of products produced above from the figure 3, it may be seen that calcining presoma in Muffle furnace under different temperatures
Al2O3Powder is unable to get α phase lower than this temperature.
As shown in Figure 4, the α-Al of different content is added into presoma2O3As crystal seed, 1050 DEG C of Muffle furnace are calcined, with
The increase of seed count, α-Al in product2O3Ratio increase, but when seed count increases to 0.839%, product is not yet
It is fully converted to α phase.
As shown in Figure 5,1100 DEG C of Muffle furnaces calcine the presoma of different seed counts, when seed count is more than 0.582%
When, product is fully converted to α phase, and the good α-Al of crystallinity can not be obtained lower than this content or lower than this temperature2O3Powder.
It will be appreciated from fig. 6 that microwave calcination does not add α-Al at 1100 DEG C2O3The presoma powder of crystal seed, with soaking time
Extension, α-Al in product2O3Ratio increase, but keep the temperature 50min product be not fully converted to α phase yet；
As shown in Figure 7, microwave calcination does not add α-Al at 1100 DEG C2O3The presoma powder of crystal seed, produces at such a temperature
Object is α-Al2O3, but XRD diffraction maximum is not sharp enough when heat preservation 10min, illustrates that product crystallinity is bad, extends soaking time extremely
30min can obtain the good α-Al of crystallinity2O3Powder.
Experimental example 2
Electronic Speculum test is scanned to embodiment 1, comparative example 3~4, comparative example 12 and comparative example 15 respectively and granularity is surveyed
Examination, tests resulting SEM figure and particle size distribution figure is shown in Fig. 8~12.It is 1200 DEG C of the Muffle furnace pure precursor preparations of calcining by Fig. 8 a
α-Al2O3Powder, average grain diameter 197nm, Fig. 9 a are the α-Al of 1300 DEG C of the Muffle furnace pure precursor preparations of calcining2O3Powder,
Average grain diameter is 262nm, and the two raising of temperature compared to known to will cause product particle size increase, reunite and increase；Figure 10 a is
1100 DEG C of calcining seeds contents of Muffle furnace are the 0.582% α-Al for driving body preparation2O3Powder, average grain diameter 165nm, with Fig. 8 a
Reduced compared to particle size, dispersibility is more preferable；Figure 11 a is that 1150 DEG C of the microwave pure presomas of calcining keep the temperature 10min preparation
α-Al2O3Powder, average grain diameter 93nm, particle size is not uniform enough, and crystallinity is bad；Figure 12 a is that 1150 DEG C of calcinings of microwave are brilliant
Kind content is the α-Al that 0.582% presoma keeps the temperature 30min preparation2O3Powder, average grain diameter 105nm, with Fig. 8 a~11a phase
Than particle size is smaller, favorable dispersibility, and crystallization effect is good.
The specific surface area of alumina powder made from comparative example 3, comparative example 4 and comparative example 12 is measured respectively, is tied
Fruit is shown in Table 2.
The specific surface area of the alumina powder of 2 comparative example 3 of table, comparative example 4 and comparative example 12
| Sample | Comparative example 3 | Comparative example 4 | Comparative example 12 |
| BET specific surface area (m2/g) | 9.55 | 4.89 | 36.27 |
Experimental example 3
In embodiment 1 when preparing Monoaluminum monoammonium disulfate Dodecahydrate, more how obtained 12 hydrated sulfuric acid of number is recrystallized
The purity of aluminium ammonium is higher.Monoaluminum monoammonium disulfate Dodecahydrate and each impurity in Monoaluminum monoammonium disulfate Dodecahydrate crystal under difference recrystallization numbers
Content be shown in Table 3.
NH under the different recrystallization numbers of table 34Al(SO4)2·12H2Each component content in O crystal
The Monoaluminum monoammonium disulfate Dodecahydrate crystal being prepared in embodiment 1 is subjected to XRD test, test result is shown in Fig. 1.
Therefore, high purity aluminium oxide in order to obtain, in preparation α-Al in embodiment2O3When powder, it is all made of third time and recrystallizes
The Monoaluminum monoammonium disulfate Dodecahydrate obtained afterwards is as precursor powder.
Experimental example 4
The alum crystal crude product 51g being prepared in Example 1 respectively is put into 1#~7# beaker, is then added
Distilled water is dissolved (number of the solution obtained after dissolution is identical as place beaker number), in water-bath under the conditions of 70 DEG C
Stirring to dissolve completely, into solution be added alum crude product quality 4% ammonium tartrate, continue stir 15min, 70 DEG C
Under the conditions of be evaporated to crystalline membrane appearance, then crystallization is dissolved in minimum flow water；Obtained hot solution is filtered while hot, is filtered
Some insoluble matter impurity are removed, filtrate is collected；Again respectively into 1#~7# filtrate be added 0ml, 10ml, 20ml, 30ml, 40ml,
50ml, 60ml dehydrated alcohol, are vigorously stirred 5min, are then placed in mixture of ice and water, and the temperature for controlling filtrate is 1 DEG C, quiet
It sets 20min and carries out crystallization；Then it is filtered, obtained crystal is washed, then microwave heating to 60 DEG C of dry 5min,
The ammonium aluminum sulfate crystal recrystallized weighs the quality of each ammonium aluminum sulfate crystal, the results are shown in Table 4.
The yield of recrystallized product under the different dehydrated alcohol additive amounts of table 4
| Number | Alum (g) | The crystallization time (min) | Dehydrated alcohol (ml) | Yield (g) | Yield (%) |
| 1# | 51 | 20 | 0 | 36.5 | 71.56 |
| 2# | 51 | 20 | 10 | 40.3 | 79.02 |
| 3# | 51 | 20 | 20 | 44.6 | 87.45 |
| 4# | 51 | 20 | 30 | 49.5 | 97.05 |
| 5# | 51 | 20 | 40 | 48.9 | 95.88 |
| 6# | 51 | 20 | 50 | 49.6 | 97.25 |
| 7# | 51 | 20 | 60 | 49.3 | 96.67 |
Claims (10)
1. a kind of method for preparing superfine alumina powder using addition crystal seed and microwave calcination, it is characterised in that: including following
Step: by precursor powder and α-Al2O3Crystal seed is uniformly mixed, and obtains mixing；Mixing is put into auxiliary heating and heat-insulating device, then
Heating and heat-insulating device will be assisted to be put into, and microwave resonance is intracavitary, and microwave heating keeps the temperature 10~50min, room temperature to 1050~1200 DEG C
Lower natural cooling to get.
2. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: α-Al in the mixing2O3The mass percent of crystal seed is 0.1~0.85%.
3. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: in mixing, α-Al2O3The partial size of crystal seed is 100~200nm.
4. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: in mixing, the partial size of presoma powder is 3~10 μm.
5. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: before heat preservation, the heating rate of heating is 15~25 DEG C/min.
6. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: the auxiliary heating and heat-insulating device includes the cavity for being used to accommodate the mixing that insulating layer and insulating layer surround；
The insulating layer includes outer heat insulation layer and the inside holding microwave absorbing material coating that outer heat insulation layer inner wall is arranged in.
7. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: the presoma powder is Monoaluminum monoammonium disulfate Dodecahydrate, and the purity of the Monoaluminum monoammonium disulfate Dodecahydrate is 4N~5N grades.
8. the method according to claim 7 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: the preparation method of the Monoaluminum monoammonium disulfate Dodecahydrate, comprising the following steps:
1) saturated solution of the two of the aluminum sulfate containing the amount for waiting substances and ammonium sulfate is mixed, is evaporated at 60~80 DEG C
There is crystalline membrane appearance, ethyl alcohol is then added, 0~10 DEG C is cooled under stirring, stand, until crystal is precipitated completely；
2) crystal being precipitated in step 1) filtered, washed, dried, obtain alum crystal crude product；
3) alum crystal crude product is dissolved in water, then solution has been evaporated to crystalline membrane appearance at 60~80 DEG C, then
Minimal amount of water is added, dissolves crystallization just, the ammonium tartrate that alum crystal crude product quality 3~5% is then added stirs
10~20min is mixed, is filtered while hot, filtrate is collected；
4) ethyl alcohol is added into filtrate, stirs, is then stood in mixture of ice and water and is cooled to crystal and is precipitated completely；
5) crystal being precipitated in step 4) filtered, washed, dried, obtain the alum recrystallized for the first time；
6) repeat step 3)~5) carry out repeated recrystallize to get.
9. the method according to claim 8 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: in step 1) and step 4), the volume of the ethyl alcohol of addition is the 10~60% of liquor capacity.
10. the method according to claim 1 for preparing superfine alumina powder using addition crystal seed and microwave calcination, special
Sign is: the α-Al2O3The preparation method of crystal seed, comprising the following steps:
A) it is 8.0~10.0 that ammonium hydroxide is added dropwise in the aluminum salt solution that aluminium ion concentration is 0.6~1.0mol/l to pH, generates Al
(OH)3Colloid；
B) by Al obtained in step a) (OH)3Colloid settles 1~3h, and the colloid after sedimentation is carried out washing and alcohol is washed, dried,
It obtains Al (OH)3Gel；
C) by Al (OH)3Gel is calcined at 1100~1300 DEG C, keep the temperature 20~50min to get.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710552151.1A CN109205648A (en) | 2017-07-07 | 2017-07-07 | A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710552151.1A CN109205648A (en) | 2017-07-07 | 2017-07-07 | A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109205648A true CN109205648A (en) | 2019-01-15 |
Family
ID=64991150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710552151.1A Pending CN109205648A (en) | 2017-07-07 | 2017-07-07 | A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109205648A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174177A (en) * | 2020-10-13 | 2021-01-05 | 中国铝业股份有限公司 | Hydraulic alumina and preparation method thereof |
| CN112919514A (en) * | 2021-03-25 | 2021-06-08 | 常州清流环保科技有限公司 | Preparation method of high-purity calcium aluminate for producing water treatment agent by using waste anthraquinone regenerant |
| CN113200558A (en) * | 2021-04-29 | 2021-08-03 | 河南长兴实业有限公司 | Production process for producing microcrystalline alpha-alumina by microwave calcination |
| CN113479918A (en) * | 2021-08-04 | 2021-10-08 | 郑州大学 | Preparation method of nano spherical alpha-alumina powder |
| CN114180613A (en) * | 2021-12-13 | 2022-03-15 | 包头稀土研究院 | Method for preparing rare earth oxide by recycling ammonia and carbon and application of rare earth oxide |
| CN114262213A (en) * | 2022-01-11 | 2022-04-01 | 无锡特科精细陶瓷有限公司 | Preparation method of small ceramic tube based on isostatic pressing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834016A (en) * | 2005-03-18 | 2006-09-20 | 住友化学株式会社 | Process for producing fine alpha-alumina particles |
| CN102040236A (en) * | 2010-11-18 | 2011-05-04 | 中国海洋石油总公司 | Preparation method of super-purity aluminum oxide |
| CN102531014A (en) * | 2011-12-23 | 2012-07-04 | 郑州航空工业管理学院 | Mixed microwave sintering method of alpha-AL203 powder |
-
2017
- 2017-07-07 CN CN201710552151.1A patent/CN109205648A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834016A (en) * | 2005-03-18 | 2006-09-20 | 住友化学株式会社 | Process for producing fine alpha-alumina particles |
| CN102040236A (en) * | 2010-11-18 | 2011-05-04 | 中国海洋石油总公司 | Preparation method of super-purity aluminum oxide |
| CN102531014A (en) * | 2011-12-23 | 2012-07-04 | 郑州航空工业管理学院 | Mixed microwave sintering method of alpha-AL203 powder |
Non-Patent Citations (1)
| Title |
|---|
| 冯拉俊等: ""热分解法制备α-Al2O3超细粉末"", 《中国粉体与技术》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174177A (en) * | 2020-10-13 | 2021-01-05 | 中国铝业股份有限公司 | Hydraulic alumina and preparation method thereof |
| CN112919514A (en) * | 2021-03-25 | 2021-06-08 | 常州清流环保科技有限公司 | Preparation method of high-purity calcium aluminate for producing water treatment agent by using waste anthraquinone regenerant |
| CN112919514B (en) * | 2021-03-25 | 2023-12-26 | 常州清流环保科技有限公司 | Preparation method of high-purity calcium aluminate for producing water treatment agent by using waste anthraquinone regenerant |
| CN113200558A (en) * | 2021-04-29 | 2021-08-03 | 河南长兴实业有限公司 | Production process for producing microcrystalline alpha-alumina by microwave calcination |
| CN113479918A (en) * | 2021-08-04 | 2021-10-08 | 郑州大学 | Preparation method of nano spherical alpha-alumina powder |
| CN113479918B (en) * | 2021-08-04 | 2023-07-18 | 郑州大学 | Preparation method of nano spherical alpha-alumina powder |
| CN114180613A (en) * | 2021-12-13 | 2022-03-15 | 包头稀土研究院 | Method for preparing rare earth oxide by recycling ammonia and carbon and application of rare earth oxide |
| CN114180613B (en) * | 2021-12-13 | 2024-04-12 | 包头稀土研究院 | Method for preparing rare earth oxide by recycling ammonia and carbon and application of rare earth oxide |
| CN114262213A (en) * | 2022-01-11 | 2022-04-01 | 无锡特科精细陶瓷有限公司 | Preparation method of small ceramic tube based on isostatic pressing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109205648A (en) | A method of superfine alumina powder is prepared using addition crystal seed and microwave calcination | |
| CN108772093B (en) | Graphite phase carbon nitride nanosheet with high visible light activity and preparation method thereof | |
| CN106946566B (en) | Preparation method of flaky barium strontium titanate powder material | |
| CN104891542B (en) | A kind of ultra-fine α Al2O3Raw powder's production technology | |
| CN102295304A (en) | Preparation method of pseudo-boehmite and microcrystalline corundum abrasive | |
| Liu et al. | Fabrication and photoluminescence properties of hollow Gd 2 O 3: Ln (Ln= Eu3+, Sm3+) spheres via a sacrificial template method | |
| CN104478006A (en) | Preparation method of tricobalt tetraoxide mesoporous nanosheets | |
| CN104031647B (en) | A kind of preparation method of round pie europium doping vanadic acid lanthanum red fluorescence powder | |
| CN105692678B (en) | Preparation method of holmium cuprate nano powder | |
| CN108910932A (en) | A kind of method that sodium carbonate precipitating prepares narrow ditribution ultrafine yttria | |
| CN107055597B (en) | The method of cubic bismuth titanate sodium powder body is quickly prepared under a kind of low temperature | |
| CN101845668B (en) | Method for preparing nano nickel borate whiskers | |
| CN113800543B (en) | Method for accelerating hydrothermal conversion rate of aluminum hydroxide into boehmite | |
| Chen et al. | Effect of temperature on the preparation of yttrium oxide in microwave field | |
| CN104973615A (en) | Microwave burning preparation method of nano gadolinium oxide powder | |
| CN102923677B (en) | Method for preparing NbSe2 nano material | |
| CN112064104A (en) | Preparation method of high-luminous-purity two-dimensional perovskite single crystal | |
| CN104556216B (en) | A kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder | |
| CN106517319B (en) | A kind of preparation method of calcium titanate micron particles | |
| CN106268612B (en) | A kind of porous barium strontium titanate raw powder's production technology | |
| CN105036148B (en) | Preparation method for flowerlike Li2Si2O5 powder | |
| CN100534904C (en) | Method for preparing nano Al2O3 adopting salt-melting calcination process | |
| CN102716701A (en) | Method for preparing nickel-doped bismuth silicon oxide microspheres by ultrasonic spray | |
| CN107777718B (en) | A kind of Y2O3Nano-powder and preparation method thereof | |
| CN110436526A (en) | One kind quickly preparing single-phase delafossite structure CuFeO2The method of micro crystal material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190115 |