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Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure

A kind of aluminum oxide nanometer and internal mesopore technology, which is applied in the direction of aluminum hydroxide preparation, alumina/hydroxide preparation, nanostructure manufacturing, etc., to achieve the effect of wide source, low energy consumption and cost, and broad application prospects

Inactive Publication Date: 2009-08-05
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are no literatures and reports on the preparation and application of nano-γ-alumina nanopowders with intra-particle mesoporous structure at home and abroad.

Method used

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  • Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure
  • Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure
  • Preparing process of nano gamma-alumina powder with intraparticle mesoporous structure

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Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: under the magnetic stirring of 1300r / min, the concentration that will contain 4.5wt% polyethylene glycol (PEG) 400 is 0.3mol / LAlCl 3 Add the solution of the same volume as the aluminum salt A solution to the concentration of 0.6mol / L ammonium bicarbonate B solution (pH is 9.3) containing 4.6wt% polyethylene glycol (PEG) 2000 at a speed of 300 drops / minute, After the titration is completed, continue to stir for 0.5 h; centrifuge, wash 3 times with secondary water and 3 times with ethanol, dry at 80° C. for 4 h, remove surface water, and obtain a dry powder. Add the obtained dry powder into 80ml of n-butanol, after ultrasonic dispersion, reflux for 2h, distill and remove the n-butanol-water azeotrope at 93°C, when the fraction temperature rises to the boiling point of n-butanol at 117°C, After stopping the distillation and continuing to reflux for 2 h, the n-butanol was recovered by distillation under reduced pressure to obtain a loose powder.

[0027] Calc...

Embodiment 2

[0028] Embodiment 2: Under the magnetic stirring of 1000r / min will contain the Al of 4.5wt% PEG400 3+ The concentration is 0.30mol / L (AlCl 3 : NH 4 Al(SO 4 ) 2 =1:1 molar ratio) solution as the aluminum salt A solution is added into an equal volume of ammonium bicarbonate B solution (pH is 9.3) containing 4.6wt% PEG2000 with a concentration of 0.60mol / L as the aluminum salt A solution at a rate of 250 drops / minute, After the titration is completed, continue to stir for 0.5 h; centrifuge, wash 3 times with secondary water and 3 times with ethanol, dry at 80° C. for 4 h, remove surface water, and obtain a dry powder. Add the obtained dry powder into 80ml of n-butanol, after ultrasonic dispersion, reflux for 2h, distill and remove the n-butanol-water azeotrope at 93°C, when the fraction temperature rises to the boiling point of n-butanol at 117°C, After stopping the distillation and continuing to reflux for 2 h, the n-butanol was recovered by distillation under reduced pressu...

Embodiment 3

[0030] Embodiment 3: under the magnetic stirring of 1300r / min will contain the Al of 8wt% PEG400 3+ The concentration is 0.4mol / L (AlCl 3 : NH 4 Al(SO 4 ) 2 =1:1) solution as the aluminum salt A solution is added at a rate of 350 drops / min to 2 times the volume of ammonium bicarbonate B solution (pH is 9.3) containing 8wt% PEG2000 with a concentration of 0.40mol / L, and the titration is completed After that, continue to stir for 0.5h; centrifuge, wash with secondary water for 3 times, add the obtained precipitate to 80ml of n-butanol, after ultrasonic dispersion, reflux for 2h, and distill to remove 93°C n-butanol-water For azeotrope, when the distillate temperature rises to 117°C, the boiling point of n-butanol, stop the distillation, continue to reflux for 2 hours, recover n-butanol by distillation under reduced pressure, and obtain a loose powder.

[0031] Calcined at 880°C for 2.5 hours to obtain γ-Al 2 o 3 product, its particle morphology see image 3 . The surface...

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Abstract

The invention discloses a preparation method of γ-alumina nanopowder with inner mesoporous structure of particles. Surfactants and adjust the pH of the ammonium bicarbonate solution. Add the aluminum salt dropwise to the ammonium bicarbonate under magnetic stirring, and continue to stir until the reaction is complete. After separation, washing, drying, azeotropic distillation and dehydration, high-temperature calcination, the particle size distribution is relatively uniform, and the average particle size in the particle is 20-63nm, γ-Al2O3 nano-powder with intra-particle mesoporous structure, the average particle internal pore diameter is 2.8-7.4nm, and the specific surface area is locally adjustable within the range of 95-212m2 / g. The invention has the advantages of simple and convenient operation, mild production conditions, low energy consumption and low cost, and is suitable for industrialized production. The prepared alumina powder has nanometer size, γ nanocrystalline phase and mesoporous characteristics at the same time, and has broad application prospects in adsorption, separation, catalyst and its carrier, and chromatographic column materials.

Description

technical field [0001] The invention relates to a method for preparing gamma-alumina nanoparticles with an inner mesoporous structure, and belongs to the field of mesoporous inorganic nanometer materials. Background technique [0002] Nano-alumina (Al 2 o 3 ) refers to alumina products with a particle size of less than 100nm. Because of its small particle size and large specific surface area, it has high chemical activity and is widely used in artificial gemstones, reagents, catalysts and carriers, luminescent materials, electronic ceramic substrates, and aerospace field. At present, the industrial preparation of alumina powder mainly adopts methods such as the Bell method and the thermal decomposition of aluminum ammonium alum, which require special heating equipment and increase the difficulty of synthesis. However, it is difficult to effectively control the size and microstructure of particles by traditional wet chemical methods, so it is difficult to prepare real nano...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/02C01F7/30C01F7/34B82B3/00
Inventor 彭天右吴志国刘迅
Owner WUHAN UNIV
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