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Preparation method of alumina hollow microspheres
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A technology of alumina hollow and hollow microspheres, applied in alumina/aluminum hydroxide and other directions, can solve problems such as complex external environment, and achieve the effects of simple equipment requirements, simple process and large specific surface area
Inactive Publication Date: 2018-10-16
WUHAN UNIV OF TECH
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Cai et al. used this principle to prepare γ-AlOOH hollow microspheres by hydrothermal synthesis [W.Q.Cai, J.G.Yu, S.Mann, Template-free hydrothermal fabrication of hierarchically organized γ-AlOOH hollow microspheres[J].Microporous Mesoporous Mater. ,2009,122:42-47], the size of the prepared hollow microspheres can be controlled by the hydrothermal time, however, the hydrothermal reaction needs to provide a complex external environment
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Embodiment 1
[0023] A preparation method of aluminum oxide hollow microspheres, the main steps are as follows:
[0024] Step 1, rapid sol-gel preparation of γ-AlOOH solid particles: 20mmolAlCl 3 ·6H 2 O was dissolved in a mixed solvent of 4ml deionized water and 6ml absolute ethanol, and stirred evenly at 60°C; then quickly added 0.1mol propylene oxide to make it gel quickly, and the sol-gel time was completed in about 15s, which was γ-AlOOH solid particle gel;
[0025] In step 2, the above-mentioned gel was aged in isopropanol at 60°C for 48 hours, and the isopropanol was replaced every 12 hours. After drying, γ-AlOOH hollow microspheres were obtained.
Embodiment 2
[0027] A preparation method of aluminum oxide hollow microspheres, the main steps are as follows:
[0028] Step 1, rapid sol-gel preparation of γ-AlOOH solid particles: 20mmolAlCl 3 ·6H 2 O was dissolved in a mixed solvent of 4ml deionized water and 6ml absolute ethanol, and stirred evenly at 60°C; then quickly added 0.1mol propylene oxide to make it gel quickly, and the sol-gel time was completed in about 15s, which was γ-AlOOH solid particle gel. ;
[0029] Step 2, aging the above gel in isopropanol at 60°C for 48 hours, changing the isopropanol every 12 hours, and obtaining γ-AlOOH hollow microspheres after drying;
[0030] Step 3, calcining the γ-AlOOH hollow microspheres obtained above at 600°C for 2 hours to obtain γ-Al 2 o 3 hollow microspheres.
Embodiment 3
[0032] A preparation method of aluminum oxide hollow microspheres, the main steps are as follows:
[0033] Step 1, rapid sol-gel preparation of γ-AlOOH solid particles: 20mmolAlCl 3 ·6H 2 O was dissolved in a mixed solvent of 4ml deionized water and 6ml absolute ethanol, and stirred evenly at 60°C; then quickly added 0.1mol propylene oxide to make it gel quickly, and the sol-gel time was completed in about 15s, which was γ-AlOOH solid particle gel. ;
[0034] Step 2, aging the above gel in isopropanol at 60°C for 48 hours, changing the isopropanol every 12 hours, and obtaining γ-AlOOH hollow microspheres after drying;
[0035] Step 3, calcining the γ-AlOOH hollow microspheres obtained above at 900°C for 2 hours to obtain δ-Al 2 o 3 hollow microspheres.
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Abstract
The invention provides a preparation method of alumina hollow microspheres. The method comprises the following steps: adding soluble aluminum salt to a mixed solution of absolute ethyl alcohol and deionized water; sealing and uniformly mixing under certain temperature; adding a certain amount of epoxypropane to realize rapid solating-gelating; ageing gel in organic solvents such as isopropanol fora while; drying to obtain gamma-AlOOH hollow microspheres; and roasting the gamma-AIOOH hollow microspheres under different temperature to obtain the alumina hollow microspheres with different crystal forms. The method is simple in processes, low in cost, high in controllability, and easy to realize massive preparation; the prepared hollow microspheres are high in specific surface area, uniform in particle size, and high in dispersity.
Description
technical field [0001] The invention belongs to the field of inorganic functional materials and relates to a preparation method of aluminum oxide hollow microspheres. Background technique [0002] As an important industrial material, alumina is widely used in people's lives, such as: catalyst carrier, adsorbent, ceramics and abrasives. Micro-nano alumina hollow microspheres not only have the unique characteristics of high hardness, high melting point and corrosion resistance of alumina itself, but also have higher adsorption and low density due to the hollow structure. [0003] The preparation process of hollow microspheres can be roughly divided into two categories, one is the template method, and the other is the template-free method. At present, most reports focus on the template method. The templates include hard templates such as polymers, carbon spheres, inorganic materials, and metal nanoparticles, and soft templates such as micelles and droplets. However, these tem...
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