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Eta-Al2O3 microsphere and preparation method and application thereof

A microsphere, sodium aluminate technology, applied in the preparation of alkali metal aluminate/alumina/aluminum hydroxide, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of preparing dispersion To solve the problems of micron-sized spherical alumina, it can achieve the effect of excellent catalytic performance, favorable for morphology control, high repeatability and magnification.

Active Publication Date: 2019-07-30
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This is because the aluminum leached from bauxite in industry basically exists in the form of sodium aluminate, and the alkaline solution is easy to handle, but there are few dispersible ones prepared from sodium aluminate solution under mild conditions. Report on Micron Spherical Alumina

Method used

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  • Eta-Al2O3 microsphere and preparation method and application thereof
  • Eta-Al2O3 microsphere and preparation method and application thereof
  • Eta-Al2O3 microsphere and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) η-Al 2 o 3 Preparation of microspheres: Dissolve 2.46g of sodium aluminate in 30mL of deionized water, and magnetically stir at room temperature (25°C) for 15min to form a sodium aluminate solution; then use a pipette to draw 20mL of N,N-dimethyl Add formamide to the above solution, continue magnetic stirring for 1 min to form a uniform clear liquid, then seal and let stand for 20 min; filter the above precipitate, wash twice with deionized water first, and finally wash once with absolute ethanol, and then dry in the air Dry in an oven at 60°C for 12h, and finally place it in a muffle furnace, bake in air at 500°C for 2h, with a heating rate of 2°C / min, and cool naturally to room temperature to obtain η-Al 2 o 3 Microspheres.

[0045] (2) preparation of catalyst: get the η-Al of 1.0g roasting 2 o 3 Microspheres, 0.0030 g of PdCl 2 Na prepared with 0.0020 g of NaCl 2 PdCl 4 The solution was added dropwise to 0.60g of the above η-Al 2 o 3 In the microspheres...

Embodiment 2

[0048] (1) η-Al 2 o 3 Preparation of microspheres: Dissolve 1.64g of sodium aluminate in 35mL of deionized water, and magnetically stir at room temperature (25°C) for 15min to form a sodium aluminate solution; then pipette 15mL of N,N-dimethyl Add methyl formamide to the above solution, continue magnetic stirring for 1 min to form a uniform clear liquid, then seal and let stand for 30 min; filter the above precipitate, and wash twice with deionized water first, and finally once with absolute ethanol, and then in the air blast Dry in a drying oven at 60°C for 12h, and finally place it in a muffle furnace, bake it in air at 500°C for 2h, the heating rate is 2°C / min, and cool naturally to room temperature to obtain η-Al 2 o 3 Microspheres.

[0049] (2) Preparation of catalyst: the loading process is the same as in Example 1.

[0050] The resulting η-Al 2 o 3 It is a rough microsphere assembled by nanosheets, with an average diameter of 4.67μm and a specific surface area of ...

Embodiment 3

[0052] (1) η-Al 2 o 3 Preparation of microspheres: Dissolve 2.46g of sodium aluminate in 40mL of deionized water, and magnetically stir at room temperature (25°C) for 15min to form a sodium aluminate solution; then use a pipette to draw 10mL of N,N-dimethyl Add acetamide to the above solution, continue magnetic stirring for 1 min to form a uniform clear liquid, then seal and let stand for 30 min; filter the above precipitate, wash twice with deionized water first, and finally wash once with absolute ethanol, and then dry in the air Dry in a box at 60°C for 12h, and finally place it in a muffle furnace, bake in air at 500°C for 2h, the heating rate is 2°C / min, and cool naturally to room temperature to obtain η-Al 2 o 3 Microspheres.

[0053] (2) Preparation of catalyst: the loading process is the same as in Example 1.

[0054] The resulting η-Al 2 o 3 It is a rough microsphere assembled by nanosheets, with an average diameter of 3.52μm and a specific surface area of ​​331...

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Abstract

The invention discloses an eta-Al2O3 microsphere and a preparation method and application thereof. The preparation method comprises the following steps of: dissolving sodium aluminate in water to prepare a sodium aluminate solution, adding a certain amount of amide into the sodium aluminate solution, uniformly stirring to form clear liquid, and sealing and standing for a certain time for double hydrolysis to generate white precipitate; filtering to obtain the precipitate, washing, drying, and roasting to obtain the final product, namely the eta-Al2O3 microsphere. The results of a small experiment show that the eta-Al2O3 is a microsphere with an average particle diameter of 2.45-5.80 micro meters assembled by nano sheets, the specific surface area is 281.4-331.4cm <2> / g, the pore volume is0.24-0.28cm <3> / g, the average pore diameter is 3.4-4.2nm, and the surface of the microsphere is smoother along with the increase of the amide concentration; the appearance and texture properties of the eta-Al2O3 microsphere are similar to those of the microsphere of the small experiment, and the selectivity of the catalysts of all the examples is 80.5-83.9%, with no significant difference.

Description

technical field [0001] The invention belongs to the field of preparation and application of alumina, in particular to a kind of η-Al 2 o 3 The preparation method of the microsphere and its application in the field of anthraquinone hydrogenation. Background technique [0002] The hydrogenation reaction of anthraquinone is a key process for the preparation of hydrogen peroxide by the industrial anthraquinone method, and the hydrogenation catalyst is the main economic cost expenditure. Therefore, in order to reduce the cost, it is very important to prepare a high-performance and low-cost hydrogenation catalyst. At present, the anthraquinone hydrogenation unit with high efficiency is a fluidized bed. In order to meet the catalyst requirements of the fluidized hydrogenation unit, the selected catalyst should have a relatively fine particle size, good dispersibility and mechanical properties, and can make The active component Pd is highly dispersed on the surface of the catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/14C01F7/44B01J23/44B01J21/04B01J32/00B01J35/10C01B15/023
CPCC01F7/14C01F7/441B01J23/44B01J21/04C01B15/023C01P2004/32C01P2004/61C01P2006/12C01P2006/14C01P2006/16B01J35/633B01J35/615B01J35/647
Inventor 蔡卫权杨志超
Owner GUANGZHOU UNIVERSITY
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