Process for preparing rutile phase spherical nano titania

A nano-titanium dioxide, rutile phase technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of complex process, high preparation cost, application limitation, etc., and achieves simplified preparation process, simple preparation process, good monodispersity Effect

Inactive Publication Date: 2009-04-08
HEBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the above methods need to add surfactants or organic additives in the reaction process, the process is complicated, so the preparation cost is high, and its application is limited

Method used

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  • Process for preparing rutile phase spherical nano titania
  • Process for preparing rutile phase spherical nano titania

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 5.5mL TiCl to the reaction kettle 4 , distilled water 95.5mL, TiCl 4 The concentration is 0.5 mol / L, a condensing device is installed on the reaction kettle, the temperature is raised to 100°C, and the temperature rise rate of the reactant is heated to boiling at 5°C / min. The reaction was continued for 5 hours. After the reaction, it was lowered to room temperature, filtered, washed several times with distilled water, dried at 80°C for 12 hours, and the obtained powder was calcined at 200°C for 5 hours to obtain 3.9g of the product. The X-ray diffraction results show that the powder is a rutile phase, and there is no anatase diffraction peak (such as figure 1 shown), the particle size of the powder is 25nm (such as figure 2 shown).

Embodiment 2

[0015] Add 8.8mL TiCl to the reaction kettle 4 , distilled water 91mL, TiCl 4 The concentration is 0.8mol / L, and a condensing device is installed on the reactor, and the temperature is raised to 80°C, and the heating rate of the reactants to boiling is 2.5°C / min. The reaction was continued for 5 hours. After the reaction was completed, it was lowered to room temperature, filtered, washed several times with distilled water, dried at 60°C for 24 hours, and the obtained powder was calcined at 600°C for 2 hours to obtain 6.3g of the product. X-ray diffraction results show that the powder is in rutile phase, no anatase diffraction peak appears, and the particle size of the powder is 70nm.

Embodiment 3

[0017] Add 11ml TiCl to the reaction kettle 4 , distilled water 89mL, TiCl 4 The concentration is 1.0mol / L, and a condensing device is installed on the reactor, and the temperature is raised to 100°C, and the heating rate of the reactant to boiling is 3.5°C / min. The reaction was continued for 5 hours. After the reaction was completed, it was lowered to room temperature, filtered, washed several times with distilled water, dried at 80°C for 12 hours, and the obtained powder was calcined at 600°C for 3 hours to obtain 7.8g of the product. X-ray diffraction results show that the powder is in rutile phase, no anatase diffraction peak appears, and the particle size of the powder is 90nm.

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Abstract

The invention discloses a low-temperature making method of rutile-phased ball-shaped nanometer titanium oxide, which comprises the following steps: adopting titanium tetrachloride solution at certain density as reactant; boiling under normal pressure; refluxing; hydrolyzing; obtaining the sediment; washing; drying; producing grain without sintering or sintered at 200-600 deg.c to crystallize; controlling the grain size at 2-100nm; obtaining the product with good dispersity.

Description

technical field [0001] The invention relates to a method for preparing rutile-phase spherical nano-titanium dioxide, which belongs to the technical field of nano-material preparation. Background technique [0002] Nano-rutile titanium dioxide is an important inorganic material, which has the characteristics of high refractive index, high melting point, large dielectric constant, compact structure, and low optical activity, so it has strong hiding power and weather resistance. At present, the preparation of rutile phase nano titanium dioxide is one of the difficult and hot issues in the field of materials. It is generally believed that rutile phase titanium dioxide is a high-temperature stable phase, and traditional rutile phase titanium dioxide is prepared by calcining anatase titanium dioxide at a high temperature above 800 °C. The cost of this method is high, and the calcination process easily causes the agglomeration of titanium dioxide particles. Therefore, finding a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053C01G23/08
Inventor 张艳峰魏雨张萍
Owner HEBEI NORMAL UNIV
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