CN102328941A - Method for preparing nano alumina - Google Patents
Method for preparing nano alumina Download PDFInfo
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- CN102328941A CN102328941A CN201110264155A CN201110264155A CN102328941A CN 102328941 A CN102328941 A CN 102328941A CN 201110264155 A CN201110264155 A CN 201110264155A CN 201110264155 A CN201110264155 A CN 201110264155A CN 102328941 A CN102328941 A CN 102328941A
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- aluminium oxide
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- alumina
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Abstract
The invention belongs to the field of inorganic material preparation and relates to a method for preparing nano alumina, and in particular relates to a method for preparing nano alumina by using a supergravity method. Aiming at the defects in the prior art, a method, which has simple process and low cost, is safe to operate and is easy to industrial product on large scale, for preparing nano alumina is provided. The method adopted in the invention has simple process and low cost, prepared alumina has high purity and uniform particle size, and is easy to achieve large-scale industrial production.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, relate to a kind of method for preparing nano aluminium oxide, particularly a kind of hypergravity legal system is equipped with the method for nano aluminium oxide.
Technical background
Aluminum oxide is widely used, and in fields such as abrasive material, structured material, refractory materials, luminescent material, aerospace, catalyzer and carriers thereof important use is arranged all, is in great demand.Therefore, need that a kind of yardstick is controlled, form is loose, with low cost, preparation technology simple and the method for favorable reproducibility prepares alumina powder jointed material.
Industry is at present gone up main Bayer process, chemical precipitation method and the aluminium salt thermal decomposition method passed through and is produced alumina powder jointed.Aluminium salt thermal decomposition method under hot conditions, need to require special heating installation, and like a large amount of obnoxious flavoures of the normal release of exsiccated ammonium alum thermal decomposition method, is unfavorable for environmental protection.Bayer process and traditional chemical precipitation method are difficult to control the size of particle effectively and reunite; The intermediate product of its generation is for being the colloidal aluminum hydroxide precipitation; Include large quantity of moisture and hydroxyl; The effect of capillary force and hydroxyl condensation causes the alumina powder jointed generation hard aggregation of gained between particle in follow-up drying and calcination process, and has a strong impact on the microtexture and the performance of sintering powder.
CN02111001.8 discloses a kind of preparation method of alumina powder with high sinter activity; Use al inorganic salt and bicarbonate of ammonia to be raw material; Prepared Alpha-alumina through the thermolysis at high temperature of aluminium carbonate ammonium, size is less than 400nm, and this raw material route environmental pollution is little.But the aluminium oxide particles particle of this method preparation is bigger, inhomogeneous, wider distribution.
CN200310100398.8 discloses a kind of superfine alumina powder material preparation technology.This method with aluminum nitrate and ammoniacal liquor as raw material, through adding dispersion agent, sorbent material; Reductive agent and sequestrant, the γ for preparing-Al2O3 particle diameter are at 8～11nm, and α-Al2O3 particle diameter is at 42～100nm; Its raw materials cost is cheap; Improved product purity, but the auxiliary agent that adds is more, will add four kinds of organism at least.
At Acta Physico-Chimica Sinica, 1999,15 (9): 830～833 " Dispersion of Sucrose on the Surface of Alumina " but in reported that sucrose disperses at the alumina surface individual layer.
It is precursor with the aluminum nitrate that CN201010236522.3 discloses a kind of; Volatile salt or bicarbonate of ammonia are precipitation agent; Under macromolecular actings in conjunction such as biological micromolecules such as sucrose and polyalcohols, pattern is controlled, utilize hydrothermal crystallizing to synthesize the method for Nano bars of alumina.
In the microwave synthesis method of the iron lithium phosphate that the disclosed lithium ion battery composite cathode material carbon of CN200610041396.X coats, add organic carbon source, use microwave heating to prepare iron lithium phosphate.
CN200880104559.1 discloses a kind of method of utilizing microwave to make flake aluminum oxide; Use microwave as heating source; Utilize the even heating characteristics of microwave and the penetration depth that regulating frequency increases microwave, heating comes fusion and synthetic flake aluminum oxide through the mixture of dispersion grinding.
International monopoly CN01819843.0 discloses the method for preparing modified aluminium hydroxide under a kind of hypergravity condition, and the mass transfer and the micro mixing of reaction greatly strengthened in the use of hypergravity, significantly improved production efficiency and product quality.
CN200710063718.5 discloses a kind of method for preparing meso-porous alumina, and under the hypergravity condition, two liquid phase reactions through aluminum nitrate and volatile salt prepare meso-porous alumina.Need feed nitrogen and oxygen respectively during calcining.
Summary of the invention
The present invention is directed to the aluminum oxide size distribution that exists on the existing technology inhomogeneous, can not reach deficiency such as high purity, the method for preparing nano aluminium oxide that provide that a kind of technology is simple, operational safety, cost are low, is easy to industrial amplification production.Adopt method of the present invention, Processes and apparatus is simple, and is with low cost, and the aluminum oxide purity of preparing is high, particle diameter is even, and is easy to realize large-scale industrial production.
The present invention adopts following technical scheme to realize:
A kind of method for preparing nano aluminium oxide comprises the steps:
(1) with aluminum nitrate and sucrose uniform mixing by a certain percentage; Be made into colorless cleared solution, aluminum nitrate concentration circulates in the helical channel rotating bed of high speed rotating between 0.1～1.0mol/L in the solution; Drip weak base until about pH=5.5, form alumina sol;
(2) step (1) gained colloidal sol after 2～6 hours, 100～150 ℃ of following air seasonings 24～48 hours, is formed grey black look precursor through 70～90 ℃ of water-baths;
(3) step (2) gained precursor is calcined in microwave Muffle furnace, the time is 2～6 hours, obtains alumina powder, when calcining temperature is 600～800 ℃, obtains γ-Al
2O
3, when calcining temperature is 1100～1400 ℃, obtain α-Al
2O
3
The above-mentioned method for preparing nano aluminium oxide, the mol ratio of wherein said aluminum nitrate and sucrose are 0.1～1: 1.
The above-mentioned method for preparing nano aluminium oxide, wherein said weak base are one or several mixing among ammoniacal liquor, volatile salt, the bicarbonate of ammonia.
The above-mentioned method for preparing nano aluminium oxide, wherein the rotating speed of helical channel rotating bed is 600～1200rpm, circular flow is 300～500L/h.
The above-mentioned method for preparing nano aluminium oxide, wherein the heating mode of microwave Muffle furnace can be to be rapidly heated or temperature programming.
Effect of the present invention and advantage:
1) use raw material variety few, low price, cost is low, and does not introduce any foreign ion;
2) reactions step is simple, and raw material is easy to get, and does not carry out purification processes and can obtain the high aluminum oxide of purity;
3) reactor drum uses hypergravity equipment, and homogeneous reaction is easy to realize scale operation;
Use microwave calcination when 4) calcining, homogeneous heating is difficult for agglomeration.
Description of drawings
Fig. 1 is the XRD diffracting spectrum of embodiment 1 resultant gama-alumina in the method for preparing nano aluminium oxide of the present invention
Fig. 2 is the XRD diffracting spectrum of embodiment 1 resultant alumina precursor in the method for preparing nano aluminium oxide of the present invention
Fig. 3 is the TEM photo of embodiment 1 resultant gama-alumina in the method for preparing nano aluminium oxide of the present invention
Embodiment
To further explain of the present invention, but the invention is not restricted to these embodiment below in conjunction with embodiment.
Embodiment 1:
The 150g aluminum nitrate is joined in the 2L water, add 68.4g sucrose, obtain the solution that aluminum nitrate concentration is 0.2mol/L; Sucrose and aluminum nitrate mol ratio are 0.5: 1, stir until dissolving fully, change in the helical channel rotating bed and circulate; The adjusting rotating speed is 800rpm; Circular flow is the 350L/h ammonia soln of Dropwise 5 % in solution then, until about pH=5.5, stops to drip, and forms colloidal sol.Produce sol solutions, be positioned over 2h in 80 ℃ of water-baths, change 120 ℃ of following dry 36h of aeration cabinet then over to, it is as shown in Figure 1 to obtain grey black look precursor product precursor XRD figure spectrum, does not have tangible sucrose or NH among the figure
4NO
3The crystalline phase diffraction peak occurs, and dehydration reaction possibly take place sucrose in the gel combustion process, is preserved with the form of carbon.Sucrose in the precursor (or its dewatered product) and remaining NH
4NO
3Be in surperficial dispersed, be not separated with alumina precursor.With the precursor crucible of packing into, put in the microwave Muffle furnace, be incubated 3h with after the heat-up rate temperature programming to 800 of 5 ℃/min ℃, the cooling back is taken out and is obtained gama-alumina.The XRD figure spectrum of gama-alumina is as shown in Figure 2, and the TEM photo is as shown in Figure 3, can find out gama-alumina by the about 15nm of length, and the rod-shpaed particle of the about 3-4nm of width is piled up and formed the granule-morphology homogeneous.
Embodiment 2:
According to preparing aluminum oxide with embodiment 1 identical method, different is: adding the sucrose amount is 96.7g, and sucrose and aluminum nitrate mol ratio are 0.7: 1, and rotating speed is 1000rpm, and the temperature of setting during calcining is 1200 ℃, and resulting product is an Alpha-alumina.
Claims (5)
1. a method for preparing nano aluminium oxide comprises the steps:
(1) with aluminum nitrate and sucrose uniform mixing by a certain percentage; Be made into colorless cleared solution, aluminum nitrate concentration circulates in the helical channel rotating bed of high speed rotating between 0.1～1.0mol/L in the solution; Drip weak base until about pH=5.5, form alumina sol;
(2) step (1) gained colloidal sol after 2～6 hours, 100～150 ℃ of following air seasonings 24～48 hours, is formed grey black look precursor through 70～90 ℃ of water-baths;
(3) step (2) gained precursor is calcined in microwave Muffle furnace, the time is 2～6 hours, obtains alumina powder, when calcining temperature is 600～800 ℃, obtains γ-Al
2O
3, when calcining temperature is 1100～1400 ℃, obtain α-Al
2O
3
2. the method for preparing nano aluminium oxide according to claim 1, the mol ratio that it is characterized in that described aluminum nitrate and sucrose is 0.1～1: 1.
3. the method for preparing nano aluminium oxide according to claim 1 is characterized in that described weak base is one or several mixing among ammoniacal liquor, volatile salt, the bicarbonate of ammonia.
4. the method for preparing nano aluminium oxide according to claim 1, the rotating speed that it is characterized in that the helical channel rotating bed is 600～1200rpm, circular flow is 300～500L/h.
5. the method for preparing nano aluminium oxide according to claim 1, the heating mode that it is characterized in that microwave Muffle furnace can be to be rapidly heated or temperature programming.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874854A (en) * | 2012-11-05 | 2013-01-16 | 四川鑫炬矿业资源开发股份有限公司 | Preparation method of 5N high-purity nanometer alumina powder |
| CN103273434A (en) * | 2013-05-31 | 2013-09-04 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
| CN105731510A (en) * | 2016-04-15 | 2016-07-06 | 中原工学院 | Method for controllably preparing aluminum oxide powder with multiple morphologies |
| CN106868394A (en) * | 2016-12-26 | 2017-06-20 | 安徽宝恒新材料科技有限公司 | A kind of method for improving steel plate mechanical performance |
| CN108977883A (en) * | 2018-09-18 | 2018-12-11 | 武汉理工大学 | A method of porous aluminas monocrystal material is prepared using microwave sintering |
| CN110373626A (en) * | 2019-08-21 | 2019-10-25 | 重庆臻宝实业有限公司 | The aluminum oxide coating layer method for sealing of anti-plasma corrosion |
| CN110935463A (en) * | 2018-09-25 | 2020-03-31 | 中国石油化工股份有限公司 | Preparation method of hydrodemetallization catalyst |
| CN111686749A (en) * | 2019-03-13 | 2020-09-22 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN116469609A (en) * | 2023-04-29 | 2023-07-21 | 开开电缆科技有限公司 | Mineral insulated cable and preparation method thereof |
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| CN1752005A (en) * | 2005-10-25 | 2006-03-29 | 湘潭大学 | Preparation method of ultrafine active aluminium oxide |
| US7491379B2 (en) * | 2005-03-21 | 2009-02-17 | National Cheng Kung University | Method for producing nano-scale θ-phase alumina microparticles |
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| US7491379B2 (en) * | 2005-03-21 | 2009-02-17 | National Cheng Kung University | Method for producing nano-scale θ-phase alumina microparticles |
| CN1752005A (en) * | 2005-10-25 | 2006-03-29 | 湘潭大学 | Preparation method of ultrafine active aluminium oxide |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874854A (en) * | 2012-11-05 | 2013-01-16 | 四川鑫炬矿业资源开发股份有限公司 | Preparation method of 5N high-purity nanometer alumina powder |
| CN102874854B (en) * | 2012-11-05 | 2014-08-06 | 四川鑫炬矿业资源开发股份有限公司 | Preparation method of 5N high-purity nanometer alumina powder |
| CN103273434A (en) * | 2013-05-31 | 2013-09-04 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
| CN103273434B (en) * | 2013-05-31 | 2015-05-27 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
| CN105731510A (en) * | 2016-04-15 | 2016-07-06 | 中原工学院 | Method for controllably preparing aluminum oxide powder with multiple morphologies |
| CN105731510B (en) * | 2016-04-15 | 2017-03-29 | 中原工学院 | A kind of alumina powder jointed method of controllable standby different morphologies |
| CN106868394A (en) * | 2016-12-26 | 2017-06-20 | 安徽宝恒新材料科技有限公司 | A kind of method for improving steel plate mechanical performance |
| CN108977883A (en) * | 2018-09-18 | 2018-12-11 | 武汉理工大学 | A method of porous aluminas monocrystal material is prepared using microwave sintering |
| CN108977883B (en) * | 2018-09-18 | 2020-12-08 | 武汉理工大学 | Method for preparing porous alumina single crystal material by adopting microwave sintering |
| CN110935463B (en) * | 2018-09-25 | 2022-07-12 | 中国石油化工股份有限公司 | Preparation method of hydrodemetallization catalyst |
| CN110935463A (en) * | 2018-09-25 | 2020-03-31 | 中国石油化工股份有限公司 | Preparation method of hydrodemetallization catalyst |
| CN111686749A (en) * | 2019-03-13 | 2020-09-22 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN111686749B (en) * | 2019-03-13 | 2022-07-12 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN110373626A (en) * | 2019-08-21 | 2019-10-25 | 重庆臻宝实业有限公司 | The aluminum oxide coating layer method for sealing of anti-plasma corrosion |
| CN110373626B (en) * | 2019-08-21 | 2021-08-20 | 重庆臻宝实业有限公司 | Plasma corrosion resistant aluminum oxide coating hole sealing method |
| CN116469609A (en) * | 2023-04-29 | 2023-07-21 | 开开电缆科技有限公司 | Mineral insulated cable and preparation method thereof |
| CN116469609B (en) * | 2023-04-29 | 2024-01-30 | 开开电缆科技有限公司 | Mineral insulated cable and preparation method thereof |
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Application publication date: 20120125 |