Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure

A nanostructured and mild technology, applied in alumina/hydroxide preparation, nanotechnology for materials and surface science, nanotechnology, etc., can solve the complex product purification process, product microstructure damage, surface activity reduction, etc. problem, to achieve the effect of realizing product morphology, reducing formation temperature, and mild preparation reaction conditions

Inactive Publication Date: 2016-09-21
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have the following problems: generally, it is necessary to add templates, surfactants or other auxiliary reagents, which makes the purification process of the product more complicated, and the removal process of the auxiliary reagents may also cause the destruction of the microstructure of the product, which is more complicated. The important thing is that the reorganization of the surface structure often leads to the reduction of the surface activity of γ-alumina nanoma

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  • Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure
  • Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure
  • Preparation method of gamma-AlOOH and gamma-Al2O3 nanotube and nanostructure

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Embodiment 1

[0034] The preparation steps are as described in the summary of the invention, 5mol 1-butyl-2,3-dimethylimidazolium chloride ([Bdmim]Cl) ionic liquid, the reaction temperature is 130°C, and the reaction time is 10h. After the reaction, it was naturally cooled to room temperature. The product was filtered, washed with deionized water and absolute ethanol, and dried in a vacuum oven at 80° C. for 3 hours to obtain γ-alumina oxyhydroxide nanomaterials. The γ-alumina oxyhydroxide precursor was placed in a ceramic crucible, and calcined in a muffle furnace at 600° C. for 2 hours to obtain γ-alumina nanomaterials.

[0035] The obtained γ-alumina oxyhydroxide and γ-alumina are respectively orthogonal γ-alumina oxyhydroxide (JCPDS Card 21-1307) and cubic γ-alumina (JCPDS Card 50-0741). The XRD spectrum and elemental analysis are shown in the attached figure 2 And attached image 3 Shown, and energy spectrum analysis could not detect zinc. Scanning and transmission electron microsc...

Embodiment 2

[0037] Reaction condition is the same as embodiment 1, only replaces zinc nitrate with the magnesium nitrate of equimolar. XRD and electron spectrum test results of the synthesized product, as attached Figure 7 shown. The XRD pattern of the prepared product is similar to the product of Example 1, which can be attributed to the orthogonal structure of γ-AlOOH (JCPDS Card21-1307), and the results of elemental analysis with electron spectroscopy show that no magnesium element product can be detected in the product. The scanning electron microscope analysis result of product shows, product appearance is also similar to embodiment 1 product (attachment Figure 8 ).

Embodiment 3

[0039] The reaction conditions are the same as in Example 1, only the reaction temperature is increased to 150°C. After the reaction, it was naturally cooled to room temperature. The product was filtered, washed with deionized water and absolute ethanol, and dried in a vacuum oven at 80° C. for 3 hours to obtain γ-alumina oxyhydroxide nanomaterials. The γ-alumina oxyhydroxide was placed in a ceramic crucible, and calcined in a muffle furnace at 600° C. for 2 hours to obtain γ-alumina nanomaterials.

[0040] The physical phase of gained gamma-alumina oxyhydroxide and gamma-alumina is identical with embodiment 1 (attachment Figure 9 And attached Figure 11 ), but the shape is bamboo leaf-like nanoflower structure (attached Figure 10 And attached Figure 11 ).

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Abstract

Disclosed is a method for preparing gamma-AlOOH and gamma-Al2O3 through ionic-liquid-assisted hydrothermal synthesis. The method is characterized in that divalent metal ions are utilized to drive a decomposition reaction of a precursor so as to generate gamma-AlOOH in a mild condition. The method comprises main steps: 1) dissolving aluminium salt, an ionic liquid and divalent metal ions in deionized water according to different ratios, and performing uniform stirring; 2) transferring the obtained solution to a reactor and performing a reaction at different reaction temperatures for a while; 3) after the reaction is over, performing cooling to the room temperature, performing centrifugalization, performing alternate washing with deionized water and absolute ethanol, and performing drying to obtain a precursor of gamma-AlOOH; and 4) putting the precursor of gamma-AlOOH in a muffle furnace, and carrying out calcination to obtain a gamma-Al2O3 nanometer material with the identical shape. According to the method, gamma-AlOOH in the shape of a needle-shaped crystal whisker, a nanotube, and a bamboo-leaf-shaped nanometer flower and gamma-Al2O3 converted from gamma-AlOOH are synthesized. The obtained gamma-Al2O3 is relatively high in degree of crystallinity and specific surface area and has comparatively high potential of large-scale production.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials. It specifically relates to a method for ionic liquid-assisted synthesis of high specific surface area gamma-alumina oxyhydroxide under mild conditions, and as a precursor, a method for obtaining gamma-alumina with the same shape through heat treatment. The invention is expected to be used in the fields of ceramics, catalysis, optics, adsorption, separation, photoelectric transfer devices, nanometer materials and composite materials. Background technique [0002] Among many non-metal and transition metal oxide materials, alumina is widely used in the fields of catalysis, ion exchange, adsorbent and ceramics because of its abundant resources, low price, large specific surface area, good chemical stability and non-toxicity. Wide range of applications. In particular, the low-temperature stable phase of alumina, γ-alumina, has abundant hydroxyl groups on its surface, and is the most wide...

Claims

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Application Information

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IPC IPC(8): C01F7/02C01F7/30B82Y30/00B82Y40/00
CPCC01F7/02B82Y30/00B82Y40/00C01F7/30C01P2002/72C01P2004/03C01P2004/04C01P2004/13C01P2004/64C01P2006/12
Inventor 郑文君秦清
Owner NANKAI UNIV
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