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Synthesis method of N doped hollow TiO2 microspheres

A synthesis method and technology of microspheres, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve complex problems

Inactive Publication Date: 2010-08-18
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Previously synthesized N-doped TiO 2 The method requires the use of inhibitors and N dopants respectively, which is more complicated

Method used

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  • Synthesis method of N doped hollow TiO2 microspheres
  • Synthesis method of N doped hollow TiO2 microspheres
  • Synthesis method of N doped hollow TiO2 microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of N-doped hollow TiO according to the present invention 2 The synthetic method of microsphere, it comprises the following steps:

[0018] 1. Synthesis of PS emulsion: add 10.0g St, 90.0g water into 250mL reaction bottle, N 2 Stir at room temperature for 20 min under protection, then heat to 70° C., add 10.0 g of KPS aqueous solution (1%, mass fraction) and react for 12 h to obtain PS emulsion.

[0019] 2. Synthesis of PS-TiO 2 Composite microspheres: add 95.0g ethanol, 5.0g ammonia water, 5.0g PS emulsion synthesized in step 1 into a 250mL reaction bottle, add 5.0g TBT, TEA, ethanol mixed solution at 50°C for 2.5h, wherein The weight ratio of TBT, TEA, and ethanol in the mixed solution is 1.0:0.2:1.0; after the addition, continue to stir for 5 hours; centrifuge the reaction product and dry it to obtain PS-TiO 2 Composite microspheres.

[0020] 3. The PS-TiO synthesized in step 2 at 500°C 2 The composite microspheres were calcined for 2 hours, and the PS cor...

Embodiment 2

[0022] Another N-doped hollow TiO according to the present invention 2 The synthetic method of microsphere, it comprises the following steps:

[0023] 1. Synthesis of PS emulsion: add 10.0g St, 90.0g water into 250mL reaction bottle, N 2 Stir at room temperature for 20 min under protection, then heat to 70° C., add 10.0 g of KPS aqueous solution (1%, mass fraction) and react for 12 h to obtain PS emulsion.

[0024] 2. Synthesis of PS-TiO 2 Composite microspheres: add 95.0g ethanol, 2.0g ammonia water, 5.0g PS emulsion synthesized in step 1 into a 250mL reaction bottle, add 2.0g TBT, TEA, and ethanol mixed solution at 50°C for 1.0h, wherein The weight ratio of TBT, TEA, and ethanol in the mixed solution is 1.0:0.1:1.0; after the addition, continue to stir for 5 hours; centrifuge the reaction product and dry it to obtain PS-TiO 2 Composite microspheres, in which PS is the core, TiO 2 for the shell.

[0025] 3. The PS-TiO synthesized in step 2 at 500°C 2 The composite micro...

Embodiment 3

[0027] Another N-doped hollow TiO according to the present invention 2 The synthetic method of microsphere, it comprises the following steps:

[0028] 1. Synthesis of PS emulsion: add 10.0g St, 90.0g water into 250mL reaction bottle, N 2 Stir at room temperature for 20 minutes under protection, then heat to 70 ° C, add 10.0 g of KPS aqueous solution (1%, mass fraction) to react for 12 hours, and obtain PS emulsion;

[0029] 2. Synthesis of PS-TiO 2 Composite microspheres: Add 95.0g ethanol, 8.0g ammonia water, 5.0g PS emulsion synthesized in step 1 into a 250mL reaction bottle, add 8.0g TBT, TEA, ethanol mixed solution at 50°C for coating for 4h, mix The weight ratio of TBT, TEA, and ethanol in the solution is 1.0:0.4:1.0; after the addition, continue to stir for 5 hours; centrifuge the reaction product and dry it to obtain PS-TiO 2 Composite microspheres.

[0030] 3. The PS-TiO synthesized in step 2 at 500°C 2 The composite microspheres were calcined for 2 hours, and the...

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Abstract

The invention discloses a synthesis method of N doped hollow TiO2 microspheres, comprising the following steps of: adding styrene, polyvinylpyrrolidone and water in a reaction vessel for stirring under the protection of N2, heating the materials to 70 DEG C, then adding a potassium persulphate aqueous solution to the heated materials for polymerization reaction to obtain polystyrene emulsion; adding ethanol, ammonia water and the polystyrene emulsion to the reaction vessel for stirring and keeping the temperate of 50 DEG C, then adding a solution with three mixed components of TBT (1-tert-butyl-1H-tetrazol-5-yl), TEA (triethanolamine) and ethanol for carrying out TiO2 cladding polystyrene particle reaction; after finishing the addition, continuously stirring the materials for a while, carrying out the centrifugal separation and drying to obtain polystyrene-TiO2(core-shell) composite microspheres; removing the polystyrene by forging to obtain the N doped hollow TiO2 microspheres. The invention has the advantages that the TEA plays a role of an inhibitor for controlling the generation of TiO2 particles and the coating speed and also an N dopant of hollow TiO2 microspheres in the process of synthesizing the N doped hollow TiO2 microspheres.

Description

technical field [0001] The invention relates to a method for synthesizing hollow inorganic microspheres, specifically a kind of N-doped hollow TiO 2 Synthesis of microspheres. Background technique [0002] In recent years, inorganic hollow particles have become the subject of extensive research in chemistry and materials science. Among them, TiO 2 Hollow microspheres have attracted special attention, and they have important applications in photocatalysis, photochemical solar cells, and chemical sensors. Polymer-TiO by calcination and solvent dissolution 2 (Core-shell) composite microspheres remove the core to obtain hollow TiO 2 Microspheres. Anatase and rutile TiO can be obtained by adjusting the calcination conditions 2 . Polymer-TiO 2 Composite microspheres are mainly prepared by layer-by-layer self-assembly method and sol-gel method. The sol-gel method is simple and has high yield. TiO 2 The hydrolysis and polycondensation of the precursor are very fast, and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/08
Inventor 乔敏吴石山陈强沈健
Owner NANJING UNIV
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