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Preparation and application of adsorbing agent of pseudo-boehmite and gamma-Al*O* hollow microspheres

A technology of pseudo-boehmite and hollow microspheres, which is applied in the preparation of microspheres, microcapsule preparation, adsorption water/sewage treatment, etc., to achieve low additive concentration, controllable grain size and good structure reproducibility Effect

Inactive Publication Date: 2010-01-06
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Unfortunately, so far, there are few reports on the development of activated alumina adsorbents with high adsorption performance by controlling the morphology of alumina.

Method used

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  • Preparation and application of adsorbing agent of pseudo-boehmite and gamma-Al*O* hollow microspheres
  • Preparation and application of adsorbing agent of pseudo-boehmite and gamma-Al*O* hollow microspheres
  • Preparation and application of adsorbing agent of pseudo-boehmite and gamma-Al*O* hollow microspheres

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preparation example Construction

[0023] Sorbent provided by the invention, its preparation method comprises the following steps:

[0024] 1. Dissolve one of aluminum sulfate, aluminum ammonium sulfate and aluminum potassium sulfate or a mixture of any proportion in distilled water, then add urea and sodium tartrate respectively, and stir to form Al 3+ The concentration is 0.0005~0.5mol / L, urea and Al 3+ A solution with a molar ratio of 1.0 to 3.0:1.0 and a sodium tartrate concentration of 0.0005 to 0.03 mol / L, then transferred to a hydrothermal kettle, and reacted at 120 to 200°C for 5 minutes to 8 hours to obtain a hydrothermal product;

[0025] 2. After cooling and filtering the hydrothermal product, wash it with distilled water until it becomes neutral, then disperse and wash the neutral filter cake once with absolute ethanol and filter it, and then vacuum-dry the obtained filter cake at 60-100°C for 4-16 hours Obtain pseudo-boehmite (core-shell) hollow microsphere powder;

[0026] 3. Calcining the vacuu...

Embodiment 1

[0031] Weigh a certain amount of aluminum sulfate, urea and sodium tartrate respectively, mix and dissolve them in 70mL distilled water, stir well to form Al 3+ The concentration is 0.05mol / L, urea and Al 3+ A solution with a molar ratio of 2.0:1.0 and a sodium tartrate concentration of 0.01 mol / L was then transferred to a hydrothermal kettle and reacted at 165°C for 3 hours under closed hydrothermal conditions. The hydrothermal product is cooled, filtered, dispersed and washed with a small amount of absolute ethanol, filtered, and then vacuum-dried at 80°C for 6 hours to obtain alumina hydrate core-shell hollow microspheres with a particle size of 2-6 μm, see figure 1 , the XRD analysis is pseudo-boehmite phase, the average grain size is 6.4nm, and its specific surface area and pore volume are 269.1m 2 / g and 0.47cm 3 / g, the average pore diameter is 8.1nm.

[0032] Prepare 100mL and 95mg / L Congo red solution and phenol solution respectively, wherein the phenol solution is...

Embodiment 2

[0035] Weigh a certain amount of aluminum sulfate, aluminum potassium sulfate, aluminum ammonium sulfate, urea and sodium tartrate respectively, mix and dissolve them in 70ml of distilled water, and stir to form Al 3+ Concentration is 0.2mol / L (among them, aluminum sulfate, aluminum potassium sulfate and aluminum ammonium sulfate are to Al 3+ Concentration contributions were 0.1, 0.04 and 0.06mol / L), urea and Al 3+ A solution with a molar ratio of 2.5:1.0 and a sodium tartrate concentration of 0.03 mol / L was then transferred to a hydrothermal kettle and reacted at 180°C for 6 hours under closed hydrothermal conditions. The hydrothermal product was cooled, filtered, dispersed and washed with a small amount of absolute ethanol in sequence, and then dried in vacuum at 60°C for 16 hours to obtain alumina hydrate microspheres with a particle size of 1-3 μm, which were pseudoboehmite by XRD analysis. Stone phase. Then it was calcined in a static air atmosphere at 700°C for 0.5h to...

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Abstract

The invention discloses a preparation method and an application of an adsorbing agent of pseudo-boehmite and gamma-Al2O3 (nuclear shell) hollow microspheres. The method comprises the following steps: dissolving aluminum sulfate, ammonium alum and aluminum potassium sulfate or a mixture thereof in an arbitrary proportion in distilled water; then respectively adding a certain quantity of urea and sodium tartrate; after the mixture is stirred uniformly, transferring the mixture into a hydrothermal kettle to carry out hydrothermal processing; and respectively obtaining the pseudo-boehmite and the gamma-Al2O3 (nuclear shell) hollow microsphere products after hydrothermal products are naturally cooled, filtered, washed, dried in vacuum and roasted. The method has simple process, moderate condition and good ruggedness of the (nuclear shell) hollow microsphere structure. The prepared pseudo-boehmite / gamma-Al2O3 hollow microspheres have excellent adsorption performance, particularly have good adsorption and purification effects on organic dye such as Congo red in waste water, and the like and hard degraded organic matters such as phenol, and the like and can be regenerated and recycled for many times, and regenerated products have the performance of adsorbing organic pollutants.

Description

technical field [0001] The invention relates to the technical field of chemical alumina production, specifically a pseudo-boehmite and γ-Al 2 o 3 Preparation method and application of (core-shell) hollow microsphere adsorbent. Background technique [0002] Pseudoboehmite is a kind of hydrated alumina. Nano pseudoboehmite has the characteristics of large specific surface area, unsaturated surface atoms, etc., and has strong adsorption capacity. Calcination product of pseudoboehmite at 400-700℃ γ-Al 2 o 3 It is widely used as catalyst carrier, catalyst and adsorbent in petrochemical and fine chemical industries [Cai Weiquan, Yu Xiaofeng. Pseudoboehmite and γ-Al 2 o 3 Preparation Research. Advances in Chemistry, 2007, 19(9): 1322-1330]. Due to nano-pseudoboehmite / γ-Al 2 o 3 There is a close relationship between the morphology and properties of the material, and pseudo-boehmite is roasted to prepare γ-Al 2 o 3 The shape of pseudo-boehmite often does not change during t...

Claims

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Application Information

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IPC IPC(8): B01J20/08B01J20/30C02F1/28B01J13/02
Inventor 余家国蔡卫权
Owner WUHAN UNIV OF TECH
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