A preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal form

A porous hydrated alumina and graded technology is applied in the field of preparation of graded mesoporous hydrated alumina microspheres to achieve the effect of low energy consumption

Active Publication Date: 2022-04-29
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Industrially, the aluminum intermediate leached from bauxite exists in the form of sodium aluminate solution, but there are few mesoporous micron-sized spheres with controllable crystal form prepared from sodium aluminate solution under mild conditions. Alumina related reports

Method used

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  • A preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal form
  • A preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal form
  • A preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal form

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Experimental program
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Effect test

Embodiment 1

[0032] Dissolve 2.46 g of sodium aluminate in 58 mL of deionized water, and stir magnetically for 15 min at 25°C to form a sodium aluminate solution; then pipette 12 mL of formamide into the above solution, and continue magnetic stirring for 1 min to form a solution; Then the solution was quickly added to a stainless steel hydrothermal kettle lined with PTFE, placed in an oven at 25°C for hydrolysis for 2 hours, and the resulting white precipitate was filtered and washed twice with deionized water in turn. , washed once with absolute ethanol, and then dried in a blast drying oven at 60°C for 12 hours to obtain pseudo-boehmite microspheres.

[0033] as table 1 and figure 1 , Figure 8 , Figure 9 As shown, the obtained flower-like pseudo-boehmite microspheres assembled by nanosheets have an average particle size of 1.02 μm and a specific surface area of ​​154.8 m 2 / g, pore volume is 0.26cm 3 / g, the average pore size is 5.3 nm, and the pore size distribution is concentrate...

Embodiment 2

[0035]Dissolve 2.46 g of sodium aluminate in 58 mL of deionized water, and stir magnetically for 15 min at 25°C to form a sodium aluminate solution; then pipette 12 mL of formamide into the above solution, and continue magnetic stirring for 1 min to form a solution; Then the solution was quickly added to a stainless steel hydrothermal kettle lined with polytetrafluoroethylene, placed in an oven at 25°C for hydrolysis for 24 hours, and the resulting white precipitate was filtered, washed with deionized water twice, Wash with absolute ethanol once, and then dry in a blast drying oven at 60°C for 12 hours to obtain Bayerite microspheres.

[0036] as table 1 and figure 2 , Figure 8 , Figure 9 As shown, the obtained flower-shaped Bayerite microspheres assembled by nanosheets have an average particle size of 1.23 μm and a specific surface area of ​​122.8 m. 2 / g, pore volume is 0.20cm 3 / g, the average pore size is 5.3 nm, and the pore size distribution is concentrated at 3.4...

Embodiment 3

[0038] Dissolve 2.46 g of sodium aluminate in 66 mL of deionized water, and stir magnetically for 15 min at 25°C to form a sodium aluminate solution; then pipette 4 mL of formamide into the above solution, and continue magnetic stirring for 1 min to form a solution; Then the solution was quickly added to a stainless steel hydrothermal kettle lined with PTFE, put it into an oven at 25°C for hydrolysis for 2 hours, and the resulting white precipitate was filtered, washed with deionized water twice, Washed with absolute ethanol once, and then dried in a blast drying oven at 60° C. for 12 hours to obtain mixed microspheres of bayerite and pseudo-boehmite.

[0039] as table 1 and image 3 , Figure 8 , Figure 9 As shown, the obtained flower-like Bayerite and pseudo-boehmite microspheres assembled by nanosheets have an average particle size of 1.02 μm and a specific surface area of ​​103.7 m 2 / g, pore volume is 0.2cm 3 / g, the average pore size is 5.2 nm, and the pore size dis...

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Abstract

The invention relates to a preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal forms. The method comprises the following steps: quickly add a certain amount of formamide into the sodium aluminate solution, and stir evenly; then quickly add the solution into a hydrothermal kettle, heat and hydrolyze for a period of time, filter the white precipitate produced after cooling, and Washing with water and absolute ethanol in sequence to obtain a filter cake; drying the filter cake to obtain flower-like mesoporous hydrated alumina microspheres assembled from two-dimensional nanosheets in different crystal forms. The flower-shaped alumina hydrate microspheres of different crystal forms prepared by the present invention have good texture properties, and changing the hydrothermal time, hydrothermal temperature and formamide addition can make the pore structure parameters change within the following range: specific surface area 103.7~250.1m 2 / g, pore volume 0.20~0.35cm 3 / g, the average pore size is 4.3-5.4nm, and the pore size is concentrated at 3.3-5.2nm.

Description

technical field [0001] The invention belongs to the technical field of alumina preparation, and in particular relates to a preparation method of graded mesoporous hydrated alumina microspheres with controllable crystal form. Background technique [0002] Alumina hydrates of different crystal forms (pseudoboehmite, bayerite and gibbsite, etc.) and alumina are widely used in electronics, petrochemicals, refractories, ceramics, abrasives, paper, pharmaceuticals and aviation. , especially activated alumina with abundant Lewis acid sites and high surface area, is often used as a catalyst or catalyst support. In order to solve the problems of catalyst agglomeration and deactivation, friction damage and recycling loss in the heterogeneous catalytic reaction, the catalyst is usually required to have a certain particle size distribution, and the preparation of catalyst microspheres can well take into account the high surface area of ​​nanomaterials. Particle size of the material and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/14B01J13/02
CPCB01J13/02C01F7/144C01P2004/50C01P2006/12C01P2006/14C01P2006/16C01P2006/17C01P2004/03C01P2002/72
Inventor 蔡卫权杨志超李文杰
Owner GUANGZHOU UNIVERSITY
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