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Preparation method of graded mesoporous hydration aluminium oxide microsphere capable of controlling crystal forms

A pore hydrated alumina, grading technology, applied in the field of preparation of mesoporous hydrated alumina microspheres, to achieve good texture properties and high crystallinity

Active Publication Date: 2019-10-29
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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  • Preparation method of graded mesoporous hydration aluminium oxide microsphere capable of controlling crystal forms
  • Preparation method of graded mesoporous hydration aluminium oxide microsphere capable of controlling crystal forms
  • Preparation method of graded mesoporous hydration aluminium oxide microsphere capable of controlling crystal forms

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Experimental program
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Effect test

Embodiment 1

[0032] Dissolve 2.46g of sodium aluminate in 58mL of deionized water, and magnetically stir at 25°C for 15 minutes to form a sodium aluminate solution; then pipette 12mL of formamide into the above solution, and continue to magnetically stir for 1min to form a solution; Then quickly add the solution to a stainless steel hydrothermal kettle lined with polytetrafluoroethylene, put it in an oven at 25°C for 2 hours, and filter the resulting white precipitate, and wash it twice with deionized water , 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, the pore volume is 0.26cm 3 / g, the average pore diameter is 5.3nm, and the pore size distribution is concentrated a...

Embodiment 2

[0035]Dissolve 2.46g of sodium aluminate in 58mL of deionized water, and magnetically stir at 25°C for 15 minutes to form a sodium aluminate solution; then pipette 12mL of formamide into the above solution, and continue to magnetically stir for 1min to form a solution; Then quickly add the solution into a polytetrafluoroethylene-lined stainless steel hydrothermal kettle, put it in an oven at 25°C for 24 hours, and filter the resulting white precipitate, wash it twice with deionized water, Wash once with absolute ethanol, 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, the pore volume is 0.20cm 3 / g, the average pore diameter is 5.3nm, and the pore size distribution is concentrated at 3.4nm.

Embodiment 3

[0038] Dissolve 2.46g of sodium aluminate in 66mL of deionized water, and magnetically stir at 25°C for 15 minutes to form a sodium aluminate solution; then pipette 4mL of formamide into the above solution, and continue to magnetically stir for 1min to form a solution; Then quickly add the solution into a polytetrafluoroethylene-lined stainless steel hydrothermal kettle, put it in an oven at 25°C for 2 hours, and filter the resulting white precipitate, wash it twice with deionized water, Wash once with absolute ethanol, and then dry in a blast drying oven at 60° C. for 12 hours to obtain mixed microspheres of Bayerite and pseudoboehmite.

[0039] as table 1 and image 3 , Figure 8 , Figure 9 As shown, the obtained flower-shaped 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, the pore volume is 0.2cm 3 / g, the average pore diameter is 5.2nm, and the pore size distribu...

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Abstract

The invention relates to a preparation method of a graded mesoporous hydration aluminium oxide microsphere capable of controlling crystal forms. The preparation method comprises the following steps oftaking a certain formamide to quickly add a sodium aluminate solution, and evenly mixing; then quickly adding the solution into a hydrothermal kettle, heating to hydrolyze for a period of time, aftercooling, filtering generated white precipitate, adding water and absolute ethyl alcohol in sequence to clean, and obtain a filter cake; and drying the filter cake, and obtaining the flowerlike mesoporous hydration aluminium oxide microsphere with different crystal forms formed by assembling two-dimensional nanometer sheets. According to the flowerlike hydrated alumina microsphere with the different crystal forms, good texture property is achieved, hydrothermal time, a hydrothermal temperature and the formamide additive amount are changed, pore structural parameters of the microsphere can change under the following ranges: 103.7-250.1 m2 / g of a specific surface area, 0.20-0.35 cm3 / g of the pore volume and 4.3-5.4 nm of the average pore diameter, and concentration distribution of pore diameters is 3.3-5.2 nm.

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 forms. Background technique [0002] Alumina hydrates of different crystal forms (pseudoboehmite, bayerite, gibbsite, etc.) and alumina are widely used in the fields of electronics, petrochemicals, refractory materials, ceramics, abrasives, papermaking, pharmaceuticals, and aviation. , especially activated alumina, which has abundant Lewis acid sites and high surface area, is often used as catalyst or catalyst support. In the heterogeneous catalytic reaction, in order to solve the problems of catalyst agglomeration deactivation, friction damage and recovery loss, etc., the catalyst is usually required to have a certain particle size distribution, and the preparation of catalyst microspheres can be very good at taking into account the characteristics of the hig...

Claims

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Application Information

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Patent Type & Authority Applications(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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