CN103449492A - Low-cost nano aluminum oxide powder preparation method and nano aluminum oxide powder - Google Patents
Low-cost nano aluminum oxide powder preparation method and nano aluminum oxide powder Download PDFInfo
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- CN103449492A CN103449492A CN2013100142578A CN201310014257A CN103449492A CN 103449492 A CN103449492 A CN 103449492A CN 2013100142578 A CN2013100142578 A CN 2013100142578A CN 201310014257 A CN201310014257 A CN 201310014257A CN 103449492 A CN103449492 A CN 103449492A
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Abstract
The invention discloses a low-cost nano aluminum oxide powder preparation method which comprises the following steps: 1. preparing an aluminum ammonium sulfate crystal from an aluminum oxide spent catalyst or aluminum scrap turnings; 2. weighing aluminum ammonium sulfate and ammonium bicarbonate, respectively preparing water solutions with deionized water, slowly and dropwisely adding a NH4Al(SO4)2 solution into a NH4HCO3 mixed solution containing a certain amount of polyethyleneglycol according to a certain mol ratio at constant temperature while stirring, adding ammonia water to regulate the pH value, aging for 0.5-10 hours after the reaction finishes, carrying out vacuum filtration, washing with distilled water and anhydrous ethanol, and drying the precipitate to obtain an ammonium aluminum carbonate precursor; and 3. calcining the ammonium aluminum carbonate precursor at 800-1200 DEG C for 1-2 hours to obtain the nano aluminum oxide powder. By using waste as the raw material, the preparation method disclosed by the invention has the advantages of cost saving, simple production technique and not need of adding complex equipment, and can easily implement industrial production.
Description
Technical field
The present invention relates to a kind of nano alumina powder jointed preparation method, refer in particular to a kind of nano alumina powder jointed preparation method cheaply and according to this preparation method, prepare nano alumina powder jointed.
Background technology
Nano aluminium oxide is because the effect of surface effects, quantum size effect, volume effect, macro quanta tunnel effect has the character of good calorifics, optics, electricity, magnetics and chemical aspect, therefore it is widely used in the high-tech areas such as conventional industries (light industry, chemical industry, building materials etc.) and novel material, microelectronics, aerospace industry, and its application prospect is very wide.Nano alumina material is the nano material that significant application value and development prospect are arranged, and has been widely used as heat-stable material, guided missile window and high-pressure mercury lamp fluorescent tube material, computer integrate circuit substrate, high-abrasive material and bioceramic material, dispersion strengthened material etc.The application of nano alumina material is mainly manifested in the following aspects: one, nano alumina powder jointed is the raw material of manufacturing nano ceramics.Nano ceramics hard wear resistant and toughness is to a certain degree arranged is the structured material with major application prospect.Use nanometer A1
2o
3the high technology ceramics that powder is made, have certain plasticity and toughness, solved the difficult problem of brittleness of ceramics, adds 5% nano level A1 in conventional pottery
2o
3powder can improve ceramic toughness, reduces ceramic sintering temperature.Study nano ceramics, obtain the first starting material from it, the ceramic powder of nanoscale is set about.Two, nano aluminium oxide can absorb UV-light, and can produce the light wave of the wavelength relevant to size of particles under the exciting of some wavelength light; Can be used as the protection of phosphor powder layer in compact fluorescent lamp films; Also can with the compound luminescent material of making fluorescent tube bulb of fluorescent RE powder, improve lamp tube service life; α-Al
2o
3can sinter crystalline ceramics into, as the material of high-pressure sodium fluorescent tube.Three, in the Industrial Catalysis agent carrier, aluminum oxide is the carrier be most widely used, and accounts for 70% of industrial loaded catalyst.The nano-alumina powder specific surface area is very large, thereby particle surface has abundant mismatch key and oxygen debt key, and the like product performance that its Performance Ratio of the catalyzer made from this and support of the catalyst is used is at present wanted more than superior several times.Therefore utilize the high-specific surface area of nanoparticle and high reactivity to promote significantly catalytic efficiency, be widely used as the catalyzer of petrochemical industry or the carrier in support of the catalyst, chemical industry novel reactor and vehicle exhaust processing.Four, the electronics crystallite is hyundai electronics industrial expansion trend.The thickness requirement of the electronic ceramics assembly of multi-layer capacitor is less than 10 μ m, and the thickness of multi layer substrate is less than 100 μ m, and good physical structure will be arranged, conventional micron A1
2o
3powder is difficult to reach requirement, only has nano level A1
2o
3that powder just has is ultra-fine, composition is even, the characteristics of single dispersion, can meet the requirement of micromodule.Utilize the nano aluminium oxide characteristic very responsive to humidity, high using value is arranged on temperature sensor.
In recent years, China was to nano aluminium oxide demand increase year after year, and the market outlook of nano aluminium oxide are quite optimistic.The quality of domestic nano aluminium oxide is difficult to guarantee, so most of high-quality main dependence on import of nano alumina material.
Nano alumina powder jointed, particularly without reuniting, particle diameter is less and narrow distribution, the nano alumina powder jointed purposes widely that has spherical in shape.But also exist a lot of problems in the preparation method, as: industrial scale is less, the nano aluminium oxide size distribution that most of preparation methods obtain is wider, and preparation process poor repeatability, higher to technology used, equipment requirements, production cost is higher, and the unfavorable factor such as the difficult control of operating process, and these have all caused the on the high side of nano powder.Per ton several thousand to several ten thousand yuan of the prices of common aluminum oxide powder (granularity be several micron), the price of nano powder is up to per ton more than 200,000 yuan.At present, the preparation of nano aluminium oxide mainly rests on the exploratory experiment stage, has also carried out the production of some exploratory industrialized levels, but also have a lot of basic needs of work to drop into a large amount of human and material resources, completes.Nano alumina powder jointed preparation is the emphasis of a lot of researcher researchs for many years always, is also the emphasis of nano-powder material industrialization.Thereby take the starting point that the working condition of enterprise and technique is research, it is very necessary exploring the technical process that is applicable to the suitability for industrialized production nano aluminium oxide.
Nano aluminium oxide is raw material mainly with expensive alkoxide or more expensive fine aluminium salt (as aluminum chloride, aluminum nitrate etc.) at present, and cost is high, produces less, holds at high price, and has seriously limited its application and industrialization process.
For the above-mentioned defect of prior art, be necessary to design a kind of new nano alumina powder jointed preparation method, thereby nano alumina powder jointed preparation reduce costs and can suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of nano alumina powder jointed preparation method cheaply and by this preparation method, prepared nano alumina powder jointed, this preparation method utilizes industrial waste or the cheap intermediate product nano alumina powder jointed material that raw material comes production purity to meet the requirements as an alternative.
Solving the technical scheme that technical problem of the present invention adopts is: a kind of nano alumina powder jointed preparation method cheaply is provided, and it comprises the following steps:
Perhaps, the aluminium scrap car of take bits are raw material, by aluminium scrap car bits, according to aluminium content and monoammonium sulfate mol ratio, are that 1:3～1:6 takes sample, divide and add for 3 ~ 5 times in the saturated solution of monoammonium sulfate, place 8 ~ 15 hours, allow it fully react and obtain the second solution;
By reacted described the first solution or the second solution filter, get filtrate, the filtrate heating is concentrated, and then recrystallization 3～5 times, pulverize it and dry, and obtains ammonium aluminum sulfate crystal;
Step 2, with deionized water, exsiccated ammonium alum and bicarbonate of ammonia are distributed and do not make the aqueous solution, in room temperature and under stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to the NH that contains polyoxyethylene glycol
4hCO
3mixing solutions in, and add ammoniacal liquor to regulate pH value to be 8 ~ 10, after completion of the reaction, to place 0.5 ~ 10 hour, suction filtration, and with distilled water and absolute ethanol washing, obtain aluminium carbonate ammonium precursor after precipitating drying;
Preferably, in step 1, the condition of oven dry is to dry 2～6 hours at 60 ℃.
Preferably, in step 3, calcination time is 1～2 hour.
Solving another technical scheme that technical problem of the present invention adopts is: a kind of prepare according to above-described preparation method nano alumina powder jointed is provided.
Compared with prior art, preparation method of the present invention has following several advantage:
1, because raw material is waste material and easily acquisition, not only saved cost, and improved physical environment.2, preparation method's of the present invention production technique is simple, without adding complex apparatus.3, be easy to suitability for industrialized production.
The accompanying drawing explanation
Fig. 1 is the flow process that the embodiment of the present invention prepares nano alumina powder jointed method.
The XRD figure that Fig. 2 is aluminium carbonate ammonium precursor.
Fig. 3 is that aluminium carbonate ammonium precursor is calcined the XRD figure of products therefrom under differing temps.
Fig. 4 be aluminium carbonate ammonium precursor with and under differing temps the TEM photo of calcining products therefrom.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Preparation method of the present invention utilizes industrial waste or cheap intermediate product (these cost of material cheap but plurality of impurities is arranged) the nano alumina powder jointed material that raw material comes production purity to meet the requirements as an alternative.The key problem in technology that preparation method of the present invention will solve has two: the 1) removal of impurity in raw material; 2) selection of large-scale production optimal conditions.
In preparation method of the present invention, there are two kinds of raw materials to be easy to obtain: one, the aluminum oxide spent catalyst of petroleum chemical industry (kind had is salic more than 50%, and year more than the output kiloton, major part can not be utilized and bury processing); Two, aluminium alloy processing industry aluminium scrap car bits (this kind of annual thousands of tons of of waste material in Shanghai only, make waste material with 2000 yuan per ton and process at present, wherein containing aluminium more than 90%).
With the composition of sem energy spectrum analysis raw material aluminium bits, result is as table 1.Can find out that from analytical results the aluminium content raw material is higher, if be used as waste disposal, be undoubtedly a kind of waste.In the raw material spent catalyst, main component is Al
2o
3, but also contain SiO
2, Fe
2o
3, other impurity such as CaO, NiO.
The analysis of table 1 aluminium scrap car bits material composition
Material composition analyzed is specified to minute and then designs concrete preparation method, comprise the removal of impurity and be made into tschermigite, and then the nano alumina powder jointed preparation flow of design preparation.
In conjunction with the Ammonia Production flow process, set up the whole process of utilizing aluminium scrap or spent catalyst large-scale production nano alumina material.
The aluminium scrap car of take bits are example, and its main reaction is:
2Al+4NH
4HSO
4=Al
2(SO
4)
3+2(NH
4)
2SO
4+2H
2(↑)
4NH
4HCO
3+NH
4Al(SO
4)
2·24H
2O=NH
4AlO(OH)HCO
3+3CO
2+2(NH
4)
2SO
4+25H
2O
As shown in Figure 1, the invention provides a kind of nano alumina powder jointed preparation method cheaply, it comprises the following steps:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
The aluminium scrap car of take bits (aluminium bits) be raw material: the aluminium scrap car is considered to be worth doing according to aluminium content and monoammonium sulfate mol ratio and taken sample as 1:3～1:6, consider several times in the saturated solution that adds monoammonium sulfate, placement is spent the night (8 ~ 15 hours), allows it fully react;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 3～5 times, by its pulverizing, dry 2～6 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
The preparation of step 2, Aluminum Carbonate Basic ammonium precursor
Take a certain amount of exsiccated ammonium alum and bicarbonate of ammonia and be mixed with the certain density aqueous solution with deionized water respectively, press certain mol ratio at constant temperature and under stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to and contains a certain amount of polyoxyethylene glycol (PEG(6000)) NH
4hCO
3mixing solutions in, and add a certain amount of ammoniacal liquor to regulate the pH value.After completion of the reaction, ageing 0.5-10 hour, suction filtration, and with distilled water and absolute ethanol washing.Obtain aluminium carbonate ammonium (NH after precipitating drying
4alO (OH) HCO
3, can be abbreviated as AACH) and precursor.
The preparation of step 3, nano aluminium oxide
Aluminium carbonate ammonium precursor, the lower calcining of different temperature (800 ~ 1200 ℃) 1 ~ 2 hour, is obtained to the nano alumina powder jointed of different crystal forms.
In the present invention, can with other containing aluminium waste, for example, waste alumina, thereby above-described step 1 can be alternative by following step 1:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
Take the aluminum oxide spent catalyst as raw material: spent catalyst is pulverized, according to alumina content and monoammonium sulfate mol ratio, it is 1:6～take at 1: 10 sample, several times (3 ~ 5 times) consider in the monoammonium sulfate that adds melting, react 0.5～1 hour, formation solution is dissolved in water after cooling;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 3～5 times, by its pulverizing, dry 2～6 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
Adopt Rigaku D/MAN-rB type X-ray diffractometer (XRD) to measure powder and calcine crystal formation and the composition of gained under differing temps.The pattern of powder particle is disperseed with ultrasonic instrument by the gained sample with size, and the suspension method sample preparation is placed in drying on the film carrier copper mesh that sprays carbon, adopts Jeol Co.JEM-1200EX II transmission electron microscope observation.
Fig. 2, Fig. 3 are respectively aluminium carbonate ammonium precursor and it calcines the XRD figure of gained final product under differing temps.Wherein, curve S 1 is in 250 ℃ of calcinings XRD figure of 1 hour; Curve S 2 is in 500 ℃ of calcinings XRD figure of 1 hour; Curve S 3 is in 700 ℃ of calcinings XRD figure of 1 hour; Curve S 4 is in 850 ℃ of calcinings XRD figure of 1 hour; Curve S 5 is in 1000 ℃ of calcinings XRD figure of 1 hour; Curve S 6 is in 1100 ℃ of calcinings XRD figure of 1 hour; Curve S 7 is in 1200 ℃ of calcinings XRD figure of 1 hour.And zero means δ-Al
2o
3;
mean α-Al
2o
3.
Position (2 θ) and relative intensity (I/I according to the three strongest ones peak of XRD
1), can find the PDF card corresponding with it number and material title, each diffraction peak of Fig. 2 and the typical diffraction peak of aluminium carbonate ammonium (AACH, PDF:76-1923) are consistent, so this synthetic precursor is AACH.In order to understand the phase transformation of heating and calcining process generation, be heated to the temperature insulation 1h of setting with the temperature rise rate of 10 ℃/min, the XRD figure spectrum of products therefrom is shown in Fig. 3.In heat-processed, the diffraction peak of 250-700 ℃ of appearance is invisible type peak, until 850 ℃ just are converted into δ-Al
2o
3, obvious peak value appears in 1100 ℃ of calcinings, with α-Al
2o
3(PDF:10-0173) match, intensity is very large, and crystallization is complete.The above results shows: the heating and calcining process experienced AACH be converted into δ-, α-Al
2o
3process, with the γ that is converted into introduced in document, δ, θ-Al
2o
3, finally be converted into α-Al
2o
3slightly different.
Fig. 4 be aluminium carbonate ammonium precursor with and respectively at 700 ℃, 850 ℃, 1000 ℃, the transmission electron microscope photos of 1100 ℃ and 1 hour (h) gained sample of 1200 ℃ of calcinings.By Fig. 4 (a), can be found out, the sample after aluminium carbonate ammonium precursor convection drying is cotton-shaped.Fig. 4 (b-f) shows that the product particle is reunited gradually along with calcining temperature raises, but final products therefrom is all in nano level.The electron diffraction demonstration is polycrystalline, and the product crystallization degree improves constantly.1100 ℃ of calcining gained α-Al
2o
3, though a small amount of reunion is arranged, grain diameter d50 concentrates and is distributed in 49nm, is suitable for doing the material of nano ceramics.
Below illustrate a kind of nano alumina powder jointed preparation method cheaply of the present invention etc. by obstructed embodiment.
Embodiment 1:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
Take the aluminum oxide spent catalyst as raw material: spent catalyst is pulverized, and is that 1:10 takes sample according to alumina content and monoammonium sulfate mol ratio, considers several times in the monoammonium sulfate that adds melting, reacts 1 hour, is dissolved in water after cooling;
Perhaps, the aluminium scrap car of take bits are raw material: aluminium scrap car bits are taken to sample according to aluminium content and monoammonium sulfate mol ratio as 1:3, consider several times in the saturated solution that adds monoammonium sulfate, placement is spent the night (12 hours), allows it fully react;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 3 times, by its pulverizing, dry 2 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
The preparation of step 2, Aluminum Carbonate Basic ammonium precursor
Take each 100g of exsiccated ammonium alum and bicarbonate of ammonia and be mixed with the certain density aqueous solution with deionized water respectively, after room temperature and lower stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to and contains a certain amount of polyoxyethylene glycol (PEG(6000)) NH
4hCO
3mixing solutions in, and to add a certain amount of ammoniacal liquor to regulate the pH value be 8.After completion of the reaction, place 0.5 hour, suction filtration, and with distilled water and absolute ethanol washing.Obtain aluminium carbonate ammonium (NH after precipitating drying
4alO (OH) HCO
3, can be abbreviated as AACH) and precursor.
The preparation of step 3, nano aluminium oxide
Aluminium carbonate ammonium precursor, the temperature lower calcination of 850 ℃ 2 hours, is obtained to δ-Al
2o
3nano-powder.
Embodiment 2:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
Take the aluminum oxide spent catalyst as raw material: spent catalyst is pulverized, and is that 1:8 takes sample according to alumina content and monoammonium sulfate mol ratio, considers several times in the monoammonium sulfate that adds melting, reacts 0.5 hour, is dissolved in water after cooling;
Perhaps, the aluminium scrap car of take bits are raw material: aluminium scrap car bits are taken to sample according to aluminium content and monoammonium sulfate mol ratio as 1:3, consider several times in the saturated solution that adds monoammonium sulfate, placement is spent the night (8 hours), allows it fully react;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 3 times, by its pulverizing, dry 2 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
The preparation of step 2, Aluminum Carbonate Basic ammonium precursor
Take each 100g of exsiccated ammonium alum and bicarbonate of ammonia and be mixed with the certain density aqueous solution with deionized water respectively, after at room temperature stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to and contains a certain amount of polyoxyethylene glycol (PEG(6000)) NH
4hCO
3mixing solutions in, and to add a certain amount of ammoniacal liquor to regulate the pH value be 8.After completion of the reaction, place 1 hour, suction filtration, and with distilled water and absolute ethanol washing.Obtain aluminium carbonate ammonium (NH after precipitating drying
4alO (OH) HCO
3, can be abbreviated as AACH) and precursor.
The preparation of step 3, nano aluminium oxide
Aluminium carbonate ammonium precursor, the temperature lower calcination of 1000 ℃ 2 hours, is obtained to δ-Al
2o
3nano-powder.
Embodiment 3:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
Take the aluminum oxide spent catalyst as raw material: spent catalyst is pulverized, and is that 1:10 takes sample according to alumina content and monoammonium sulfate mol ratio, considers several times in the monoammonium sulfate that adds melting, reacts 1 hour, is dissolved in water after cooling;
Perhaps, the aluminium scrap car of take bits are raw material: aluminium scrap car bits are taken to sample according to aluminium content and monoammonium sulfate mol ratio as 1:6, consider several times in the saturated solution that adds monoammonium sulfate, placement is spent the night (15 hours), allows it fully react;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 5 times, by its pulverizing, dry 6 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
The preparation of step 2, Aluminum Carbonate Basic ammonium precursor
Take each 100g of exsiccated ammonium alum and bicarbonate of ammonia and be mixed with the certain density aqueous solution with deionized water respectively, after at room temperature stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to and contains a certain amount of polyoxyethylene glycol (PEG(6000)) NH
4hCO
3mixing solutions in, and to add a certain amount of ammoniacal liquor to regulate the pH value be 10.After completion of the reaction, place 10 hours, suction filtration, and with distilled water and absolute ethanol washing.Obtain aluminium carbonate ammonium (NH after precipitating drying
4alO (OH) HCO
3, can be abbreviated as AACH) and precursor.
The preparation of step 3, nano aluminium oxide
Aluminium carbonate ammonium precursor, the temperature lower calcination of 1100 ℃ 1 hour, is obtained to α-Al
2o
3nano-powder.
Embodiment 4:
The preparation of step 1, ammonium aluminum sulfate crystal (tschermigite)
Take the aluminum oxide spent catalyst as raw material: spent catalyst is pulverized, and is that 1:10 takes sample according to alumina content and monoammonium sulfate mol ratio, considers several times in the monoammonium sulfate that adds melting, reacts 1 hour, is dissolved in water after cooling;
Perhaps, the aluminium scrap car of take bits are raw material: aluminium scrap car bits are taken to sample according to aluminium content and monoammonium sulfate mol ratio as 1:6, consider several times in the saturated solution that adds monoammonium sulfate, placement is spent the night (10 hours), allows it fully react;
By solution filter after above-mentioned reaction, get filtrate, the filtrate heating is concentrated, and recrystallization 5 times, by its pulverizing, dry 6 hours at 60 ℃, obtains ammonium aluminum sulfate crystal.
The preparation of step 2, Aluminum Carbonate Basic ammonium precursor
Take each 100g of exsiccated ammonium alum and bicarbonate of ammonia and be mixed with the certain density aqueous solution with deionized water respectively, after at room temperature stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to and contains a certain amount of polyoxyethylene glycol (PEG(6000)) NH
4hCO
3mixing solutions in, and to add a certain amount of ammoniacal liquor to regulate the pH value be 10.After completion of the reaction, place 10 hours, suction filtration, and with distilled water and absolute ethanol washing.Obtain aluminium carbonate ammonium (NH after precipitating drying
4alO (OH) HCO
3, can be abbreviated as AACH) and precursor.
The preparation of step 3, nano aluminium oxide
Aluminium carbonate ammonium precursor, the temperature lower calcination of 1200 ℃ 1 hour, is obtained to α-Al
2o
3nano-powder.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. a nano alumina powder jointed preparation method cheaply, is characterized in that, it comprises the following steps:
Step 1, take the aluminum oxide spent catalyst as raw material: by aluminum oxide spent catalyst grind into powder, according to alumina content and monoammonium sulfate mol ratio, it is 1:6～take at 1: 10 sample, divide and add for 3 ~ 5 times in the monoammonium sulfate of melting, react 0.5～1 hour, being dissolved in water after cooling obtains the first solution;
Perhaps, the aluminium scrap car of take bits are raw material, by aluminium scrap car bits, according to aluminium content and monoammonium sulfate mol ratio, are that 1:3～1:6 takes sample, divide and add for 3 ~ 5 times in the saturated solution of monoammonium sulfate, place 8 ~ 15 hours, allow it fully react and obtain the second solution;
By reacted described the first solution or the second solution filter, get filtrate, the filtrate heating is concentrated, and then recrystallization 3～5 times, pulverize it and dry, and obtains ammonium aluminum sulfate crystal;
Step 2, with deionized water, exsiccated ammonium alum and bicarbonate of ammonia are distributed and do not make the aqueous solution, in room temperature and under stirring, slowly by NH
4al (SO
4)
2solution is added drop-wise to the NH that contains polyoxyethylene glycol
4hCO
3mixing solutions in, and add ammoniacal liquor to regulate pH value to be 8 ~ 10, after completion of the reaction, to place 0.5 ~ 10 hour, suction filtration, and with distilled water and absolute ethanol washing, obtain aluminium carbonate ammonium precursor after precipitating drying;
Step 3, the aluminium carbonate ammonium precursor in the temperature lower calcination step 2 of 800 ~ 1200 ℃, obtain nano alumina powder jointed.
2. preparation method according to claim 1, is characterized in that, in step 1, the condition of oven dry is to dry 2～6 hours at 60 ℃.
3. preparation method according to claim 1, is characterized in that, in step 3, calcination time is 1～2 hour.
4. prepare according to the described preparation method of claims 1 to 3 any one nano alumina powder jointed.
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| CN108706617A (en) * | 2018-06-21 | 2018-10-26 | 沈阳工业大学 | A method of comprehensive utilization aluminium ash |
| CN111410220A (en) * | 2020-04-28 | 2020-07-14 | 山东国瓷功能材料股份有限公司 | Low-dielectric-constant high-thermal-conductivity alumina material for high-frequency application and preparation method thereof |
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| CN108706617A (en) * | 2018-06-21 | 2018-10-26 | 沈阳工业大学 | A method of comprehensive utilization aluminium ash |
| CN108706617B (en) * | 2018-06-21 | 2020-05-22 | 沈阳工业大学 | Method for comprehensively utilizing aluminum ash |
| CN111410220A (en) * | 2020-04-28 | 2020-07-14 | 山东国瓷功能材料股份有限公司 | Low-dielectric-constant high-thermal-conductivity alumina material for high-frequency application and preparation method thereof |
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