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Process for preparing rutile phase spherical nano TiO2

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

Inactive Publication Date: 2007-08-01
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 TiO2

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 5.5mL TiCl to the reactor 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 at which the reactant is heated to boiling is 5°C / min. The reaction was continued for 5 hours. After the reaction, it was cooled to room temperature, filtered, washed with distilled water several times, and dried at 80°C for 12 hours. The obtained powder was calcined at 200°C for 5 hours to obtain 3.9g of product. X-ray diffraction results show that the powder is rutile phase, no anatase diffraction peak appears (as shown in Figure 1), and the particle size of the powder is 25 nm (as shown in Figure 2).

Embodiment 2

[0015] Add 8.8mL TiCl to the reactor 4 , Distilled water 91mL, TiCl 4 The concentration is 0.8 mol / L, a condensing device is installed on the reaction kettle, the temperature is raised to 80°C, and the heating rate of the reactant is heated to boiling at 2.5°C / min. The reaction was continued for 5 hours. After the reaction, it was cooled to room temperature. After filtration, it was 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 6.3 g of product. X-ray diffraction results show that the powder is rutile, no anatase diffraction peak appears, and the particle size of the powder is 70 nm.

Embodiment 3

[0017] Add 11ml TiCl to the reactor 4 , Distilled water 89mL, TiCl 4 The concentration is 1.0 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 heated to boiling is 3.5°C / min. The reaction was continued for 5 hours. After the reaction, the temperature was lowered to room temperature. After filtration, it was washed several times with distilled water and dried at 80°C for 12 hours. The obtained powder was calcined at 600°C for 3 hours to obtain 7.8 g of product. X-ray diffraction results show that the powder is rutile, 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, and belongs to the technical field of nano material preparation. Background technique [0002] Nano-rutile titanium dioxide is an important inorganic material. It 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-titania is one of the difficult and hot issues in the material field. It is generally believed that the rutile phase titanium dioxide belongs to the high temperature stable phase, and the traditional rutile phase titanium dioxide is prepared by calcination of anatase titanium dioxide at a high temperature above 800°C. The method has high cost, and the calcination process easily causes agglomeration of titanium dioxide particles. Therefore, finding a method to direc...

Claims

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Application Information

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IPC IPC(8): C01G23/053C01G23/08
Inventor 张艳峰魏雨张萍
Owner HEBEI NORMAL UNIV
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