Method of preparing hollow mesoporous zirconium dioxide through sol-gel protective method

A technology of zirconia and protection method, which is applied in the field of preparation of hollow mesoporous zirconia, which can solve the problems of poor stability and easy breakage of mesoporous zirconia materials, and achieve the effect of regular shape and corrosion inhibition

Inactive Publication Date: 2016-07-06
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] ShaohengTang, XiaoqingHuang et al. 2 Nanospheres are templates, zirconium n-butoxide is the source of zirconium, and hollow mesoporous zirconia nanomaterials are prepared by the hard template method, but the mesoporous zirconia materials prepared by this method are extremely fragile, especially for large-walled cavities. Thin microspheres are less stable

Method used

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  • Method of preparing hollow mesoporous zirconium dioxide through sol-gel protective method
  • Method of preparing hollow mesoporous zirconium dioxide through sol-gel protective method
  • Method of preparing hollow mesoporous zirconium dioxide through sol-gel protective method

Examples

Experimental program
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Embodiment 1

[0022] Example 1: 44mL ethanol, 2mL ammonia water, and 9mL water were stirred at 30°C and 300rpm for 30 minutes, then added 4mLTEOS, reacted for 8 hours, centrifuged, washed with water and ethanol to obtain monodisperse SiO with a thickness of about 100nm 2 Microspheres; the product is dispersed in 180mL of ethanol, at 30°C, at a speed of 400rpm, add 0.3mL of Brij30, 0.3mL of water and 1.3mL of zirconium n-butoxide, react for 8h, centrifuge, wash with water, the product is dispersed in 40mL of water, and aged for 12h Disperse the product in 80mL of water, add 0.15g of PVP at 400rpm, react for 24h, centrifuge, wash with ethanol; disperse the appeal product in 44mL of ethanol, 2mL of ammonia water, 9mL of water at 30°C and 300rpm, stir for 30min, Add 4mLTEOS, react for 8h, centrifuge, wash with water and ethanol to obtain monodisperse SiO 2 ZrO 2 SiO 2 Particles; calcined at 600°C for 5h; the above product was denucleated with an aqueous solution of NaOH, centrifuged, washed, ...

Embodiment 2

[0023] Example 2: 75mL ethanol, 5.13mL ammonia water, and 8mL water were stirred at a temperature of 30°C and a speed of 300rpm for 30 minutes, then 6mLTEOS was added, reacted for 8h, centrifuged, washed with water and ethanol to obtain monodisperse SiO of about 300nm 2 Microspheres; the product is dispersed in 180mL ethanol, at 30°C and 400rpm, add 0.5mL Brij30, 0.5mL water and 1.5mL zirconium n-butoxide, react for 8h, centrifuge, wash with water, disperse the product in 40mL water, and age for 12h Disperse the product in 80mL of water, add 0.15g of PVP at 400rpm, react for 24h, centrifuge, wash with ethanol; disperse the product in 75mL of ethanol, 5.13mL of ammonia water, 8mL of water at 30°C and 300rpm, stir for 30min , add 6mLTEOS, react for 8h, centrifuge, wash with water and ethanol to get monodisperse SiO 2 ZrO 2 SiO 2 Particles; calcined at 600°C for 5h; the above product was denucleated with an aqueous solution of NaOH, centrifuged, washed, and dried to obtain mono...

Embodiment 3

[0024] Example 3: 91mL ethanol, 32.5mL ammonia water, at a temperature of 30°C and a speed of 300rpm, after stirring for 30min, add 5.5mLTEOS, react for 1h, centrifuge, wash with water and ethanol to obtain monodisperse SiO of about 500nm 2 Microspheres; the product is dispersed in 175mL ethanol, at 30°C and 400rpm, add 0.13mL Brij30, 0.13mL water and 1.0mL zirconium n-butoxide, react for 8h, centrifuge, wash with water, disperse the product in 40mL water, and age for 12h Disperse the product in 80mL of water, add 0.15g of PVP at 400rpm, react for 24h, centrifuge, wash with ethanol; disperse the product in 75mL of ethanol, 5.13mL of ammonia water, 8mL of water at 30°C and 300rpm, stir for 30min , add 3mLTEOS, react for 8h, centrifuge, wash with water and ethanol to get monodisperse SiO 2 ZrO 2 SiO 2 Particles; calcined at 600°C for 5h; the above product was denucleated with an aqueous solution of NaOH, centrifuged, washed, and dried to obtain monodisperse hollow mesoporous z...

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Abstract

The invention discloses a method of preparing hollow mesoporous zirconium dioxide through a sol-gel protective method. The method includes the steps of: 1) synthesis of mono-dispersed silicon dioxide microsphere seeds through a Stober method: adding a certain amount of TEOS to a solvent system comprising alcohol, water and ammonia water at the reaction temperature of 30 DEG C to obtain the mono-dispersed silicon dioxide microsphere seeds; 2) dispersing the mono-dispersed silicon dioxide microsphere seeds in an alcohol system, adding a certain amount of a mesoporous agent, water and a zirconium source at the reaction temperature of 30 DEG C, performing centrifugation, and washing and aging the mixture and adding a certain amount of a template agent to prepare mono-dispersed mesoporous SiO2@ZrO2 microspheres; 3) at the reaction temperature of 30 DEG C, placing the microspheres in the system comprising alcohol, water and ammonia water through the sol-gel protective method, adding a certain amount of TEOS, centrifugally washing, drying and calcining the mixture to prepare mono-dispersed SiO2@ZrO2@SiO2 microspheres; and 4) dispersing the microspheres in a sodium hydroxide water solution, stirring the mixture to remove the cores to obtain the mono-dispersed hollow mesoporous zirconium dioxide microspheres. The hollow mesoporous zirconium dioxide, as an excellent nano container, is used for adsorbing and pH-controllably releasing a corrosion inhibitor to inhibit corrosion.

Description

technical field [0001] The invention belongs to the technical field of production of spherical powder materials, and in particular relates to a method for preparing hollow mesoporous zirconia by a sol-gel protection method. Background technique [0002] According to comprehensive literature reports, hollow microspheres have important applications in many fields such as chemistry, biology and materials, such as for the preparation of controlled release capsules (drugs, pigments, cosmetics, inks, etc.), electrical components, lightweight fillers, catalysts and Carrier, separation material, sound insulation material, etc. [0003] Mesoporous material is a new type of material with a pore size between micropores and macropores, which has a huge surface area and a three-dimensional pore structure. The research and development of mesoporous materials are of great significance for both theoretical research and practical production. It has excellent characteristics that other poro...

Claims

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Application Information

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IPC IPC(8): C01G25/02B01J13/02B01J20/06B01J20/30
Inventor 傅佳骏刘梦阳刘影王明东孙广平
Owner NANJING UNIV OF SCI & TECH
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