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Method for preparing dual-shell hollow micro-nano structural TiO2 microspheres by one-step template-hydrothermal process

A micro-nano structure, double-shell technology, applied in the direction of titanium oxide/hydroxide, titanium dioxide, etc., can solve the problems of high fault tolerance, necessity of complex multi-step synthesis process, cumbersome operation process, etc., to achieve simple operation and save The effect of simple resources and processes

Inactive Publication Date: 2018-04-13
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the above template method has been proven to successfully prepare double-shell hollow TiO 2 Microspheres, but there are some shortcomings, mainly reflected in: 1) the necessity of a complex multi-step synthesis process; 2) the operation process is cumbersome and the error tolerance rate is too high

Method used

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  • Method for preparing dual-shell hollow micro-nano structural TiO2 microspheres by one-step template-hydrothermal process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The following are parts by mass,

[0027] Weigh 15 parts glucose and 1 part (NH 4 ) 2 TiF 6 , dissolved in a certain amount of deionized water, and stirred evenly; the mixture was transferred into a hydrothermal kettle, reacted at 190 °C for 24 hours, and washed several times by centrifugation to obtain black powder; finally, the black powder was treated at high temperature in a muffle furnace, After calcining at 550 °C for 4 h, the white powder was collected, that is, the double-shelled hollow micro-nano-structured TiO 2 Microspheres.

Embodiment 2

[0029] The following are parts by mass,

[0030] Weigh 20 parts of glucose and 2 parts (NH 4 ) 2 TiF 6 , dissolved in a certain amount of deionized water, and stirred evenly; the mixture was transferred into a hydrothermal kettle, reacted at 190 °C for 20 hours, and washed several times with centrifugal water to obtain black powder; finally, the black powder was treated at high temperature in a muffle furnace, After calcining at 550 °C for 4 h, the white powder was collected, that is, the double-shelled hollow micro-nano-structured TiO 2 Microspheres.

Embodiment 3

[0032] The following are parts by mass,

[0033] Weigh 30 parts of glucose and 1 part (NH 4 ) 2 TiF 6 , dissolved in a certain amount of deionized water, and stirred evenly; the mixture was transferred into a hydrothermal kettle, reacted at 190 ° C for 18 hours, and washed several times by centrifugation to obtain black powder; finally, the black powder was processed in a muffle furnace at high temperature, After calcining at 550 °C for 4 h, the white powder was collected, that is, the double-shelled hollow micro-nano-structured TiO 2 Microspheres.

[0034] see figure 1 ,from figure 1 It can be seen from the left and right of the double-shelled hollow micro-nano-structured TiO that can be successfully prepared by a one-step template-hydrothermal method. 2 The particle size of the inner shell is about 400nm, and the particle size of the outer shell is about 1-1.5μm. The hollow structure is obvious, and each sphere is in a monodispersed state with regular morphology.

[...

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Abstract

The invention relates to a method for preparing dual-shell hollow micro-nano structural TiO2 microspheres by one-step template-hydrothermal process. The method comprises: weighing 15-30 parts of glucose and 1-3 parts of ammonium hexafluorotitanate ((NH4)2TiF6), dissolving in certain deionized water, and stirring well; moving the mixed liquid into a hydrothermal kettle, allowing reacting at 190 DEGC for 18-24 h, and centrifugally washing with water several times to obtain black powder; treating the black powder at a high temperature in a muffle furnace, calcining at the temperature of 550 DEGC for 4 h, and collecting white powder that is dual-shell hollow micro-nano structural TiO2 microspheres. The method of the invention has the advantages that the traditional complex operations to prepare dual-shell hollow structures, such as multi-template assist, multi-coating and selective etching, the process is simple and feasible, and the raw materials are low in price and easy to obtain; inaddition, no surfactants are involved in the reaction, and contamination by organic solvents in the prior art such as auxiliary stabilizers, pore-forming agents and foaming agents and a series of posttreatment problems caused by the contamination can be avoided.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing double-shelled hollow micro-nano-structured TiO2 microspheres by a one-step template-hydrothermal method. Background technique [0002] At present, the synthesis method of double-shell hollow microspheres is relatively simple. Generally, the hard template method is used to obtain double-shell hollow structure microspheres by layer-by-layer coating through multi-step reactions. The basic principle is to use the force between the titanium source precursor and the template agent, such as electrostatic interaction, hydrogen bond, covalent bond, etc. 2 It is deposited on the surface of the template to obtain a coating structure, and then the template agent is removed by calcination or extraction to obtain a single-shell hollow structure nano-TiO 2 microspheres, further by a similar operation on TiO 2 A template agent is deposited on th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047
CPCC01G23/047C01P2004/34C01P2004/61C01P2004/62
Inventor 吕斌程坤高党鸽马建中
Owner SHAANXI UNIV OF SCI & TECH
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