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Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor

A technology of zinc orthotitanate and hydrotalcite, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve problems such as poor product component uniformity, poor component uniformity, and precipitation speed difference, and achieve crystallinity and Good component uniformity, large grain size, and the effect of lowering the calcination temperature

Inactive Publication Date: 2013-03-13
SHANDONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies of the prior art, the present invention provides a method for preparing nano-zinc orthotitanate spinel using zinc-titanium hydrotalcite as a precursor, which solves the problems of incomplete reaction and poor product component uniformity in traditional ceramic methods; In the method of the invention, metal inorganic salts are used as reactants, which overcomes unfavorable factors such as high preparation cost in the sol-gel method, danger of calcination and unfriendly environment; in the method of the invention, the precursor is prepared by urea hydrolysis, avoiding the The liquid phase deposition method has the disadvantages of differences in precipitation speed and poor uniformity of each component

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  • Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor
  • Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor

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Embodiment 1

[0035] A method for preparing nano-zinc orthotitanate spinel with zinc-titanium hydrotalcite as precursor, the method comprises the following steps:

[0036] (1) Preparation of zinc-titanium hydrotalcite precursor

[0037] Measure 4.40mlTiCl 4 Dissolve in 200ml deionized water to obtain titanium solution, weigh 23.80gZn(NO 3 ) 2 ·6H 2 O and 21.60gCO(NH 2 ) 2 Dissolved in the titanium solution to obtain a mixed salt solution, Zn in the solution 2+ : Ti 4+ The molar ratio is 2, CO(NH 2 ) 2 :(Zn 2+ +Ti 4+ ) molar ratio is 3, where Zn(NO 3 ) 2 ·6H 2 O molar concentration is 0.4mol / L, TiCl 4 The molar concentration is 0.2mol / L, CO(NH 2 ) 2 The molar concentration is 1.8mol / L; transfer the mixed salt solution to a three-neck flask and immerse the three-necked flask in a 100°C oil bath, stir and heat for 24 hours, keep the oil bath temperature at 100°C for 12 hours, and cool to room temperature Filter and rinse twice with deionized water, and finally dry at 60°C for ...

Embodiment 2

[0042] A method for preparing nano-zinc orthotitanate spinel with zinc-titanium hydrotalcite as precursor, the method comprises the following steps:

[0043] (1) Preparation of zinc-titanium hydrotalcite precursor

[0044] Measure 2.20mlTiCl 4 Dissolve in 200ml deionized water to obtain titanium solution, weigh 17.25gZn(NO 3 ) 2 ·6H 2 O and 14.4gCO(NH 2 ) 2 Dissolved in the titanium solution to obtain a mixed salt solution, Zn in the solution 2+ : Ti 4+ The molar ratio is 3, CO(NH 2 ) 2 :(Zn 2+ +Ti 4+ ) molar ratio is 3, where Zn(NO 3 ) 2 ·6H 2 O molar concentration is 0.3mol / L, TiCl 4 The molar concentration is 0.1mol / L, CO(NH 2 ) 2 The molar concentration is 1.2mol / L; transfer the mixed salt solution to a three-necked flask and immerse the three-necked flask in a 100°C oil bath to stir and heat for 24 hours, then stand at the same temperature for 12 hours, cool to room temperature, filter and use Rinse with deionized water three times, and finally dry at 70°...

Embodiment 3

[0049] A method for preparing nano-zinc orthotitanate spinel with zinc-titanium hydrotalcite as precursor, the method comprises the following steps:

[0050] (1) Preparation of zinc-titanium hydrotalcite precursor

[0051] Measure 0.88mlTiCl 4 Dissolve in 200ml deionized water to obtain titanium solution, weigh 2.18g ZnCl 2 and 7.2gCO(NH 2 ) 2 Dissolved in the titanium solution to obtain a mixed salt solution, Zn in the solution 2+ : Ti 4+ The molar ratio is 2, CO(NH 2 ) 2 :(Zn 2+ +Ti 4+ ) in a molar ratio of 5, where ZnCl 2 The molar concentration is 0.08mol / L, TiCl 4 The molar concentration is 0.04mol / L, CO(NH 2 ) 2 The molar concentration was 0.6mol / L; the mixed salt solution was transferred to a three-necked flask and the three-necked flask was immersed in a 100°C oil bath and stirred and heated for 12 hours, then stood at the same temperature for 12 hours, cooled to room temperature, filtered and used Rinse with deionized water 4 times, and finally dry at 60°...

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Abstract

The invention relates to a method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as a precursor, and the method comprises the following steps of (1): weighing a bivalent zinc salt, a tetravalent titanium salt and CO (NH2)2 and adding deionized water to obtain a mixed salt solution, carrying out oil-bath heating at the temperature of 70-110 DEG C, stirring, cooling, and grinding a filter cake, thereby obtaining the zinc-titanium hydrotalcite precursor; and (2) putting the obtained zinc-titanium hydrotalcite precursor in a muffle furnace, heating to 600-1000 DEG C, performing heat preservation, and cooling to the room temperature, thereby obtaining the Zn2TiO4 spinel. The method disclosed by the invention has the advantages that the lamellar zinc-titanium hydrotalcite precursor is prepared by utilizing a urea hydrolysis method; the pH (potential of Hydrogen) value is not needed to be adjusted; the obtained precursor is large in grain size and better in crystallinity and dispersity; and the obtained Zn2TiO4 spinel is uniform in constituent and small in granularity.

Description

technical field [0001] The invention relates to a preparation method of nano-zinc orthotitanate spinel, in particular to the preparation of nano-zinc orthotitanate (Zn 2 TiO 4 ) spinel method. Background technique [0002] Zinc orthotitanate spinel is a widely used inorganic non-metallic material. It was mainly used as white pigment or paint at first. Later, zinc titanate was found to be used in high temperature desulfurization adsorbent, microwave dielectric ceramic, catalyst carrier and ultraviolet shielding and other fields have important application potential. At present, the methods for preparing such spinel mainly include ceramic method, sol-gel method, liquid phase deposition method and so on. The ceramic method requires a higher calcination temperature, which is not conducive to production and energy saving; the product is easy to agglomerate during calcination, the overall uniformity is poor, and the specific surface area is small. The sol-gel method generally u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00B82Y30/00
Inventor 刘建强姜海辉宋箭叶冷明哲覃耀慰
Owner SHANDONG UNIV