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Method for preparing hano-level titanium dioxide by controlling crystal form

A titanium dioxide, nano-scale technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of limitation and high cost of raw materials, and achieve the effect of process operation, uniform particle size and simple method

Inactive Publication Date: 2006-08-09
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is feasible, the cost of raw materials is relatively high, which is limited in industrial production.

Method used

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  • Method for preparing hano-level titanium dioxide by controlling crystal form
  • Method for preparing hano-level titanium dioxide by controlling crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the titanyl sulfate deionized water, slowly add 5mol / L sodium hydroxide solution, the whole process controls the reaction temperature to not exceed 40℃, and terminates when the pH is 5; filter and wash twice with deionized water to 0.1mol / L BaCl 2 Solution can not detect SO 4 2- Add 6mol / L hydrochloric acid under stirring conditions to dissolve the resulting filter cake, and control the temperature at 20°C. When it is completely dissolved, stop adding acid; add 2.5% potassium citrate, and hydrolyze at 95°C for 1 hour, The product is filtered, washed with deionized water twice, dried at 100°C, and then moved into a muffle furnace and calcined at 700°C for 1.5 hours to obtain mixed crystal titanium dioxide powder with 75% rutile and 25% anatase.

[0026] X-ray diffraction pattern such as figure 1 (b) Shown.

Embodiment 2

[0028] In the titanyl sulfate deionized water, slowly add 5mol / L sodium carbonate solution, the whole process controls the reaction temperature not to exceed 40℃, and terminates when the pH is 7; filter and wash to 0.1mol / L BaCl 2 Solution can not detect SO 4 2- Add 3mol / L hydrochloric acid under stirring conditions to dissolve the resulting filter cake, and control the temperature at 10℃, when it is completely dissolved, stop adding acid; add 5% sodium citrate, and hydrolyze at 105℃ for 0.5h The product is filtered, washed, dried at 120°C, moved into a muffle furnace and calcined at 650°C for 1.5 hours to obtain mixed crystal titanium dioxide powder with 50% rutile and 50% anatase.

[0029] X-ray diffraction pattern such as figure 1 As shown in (c), the SEM image of the obtained sample is as figure 2 Shown.

Embodiment 3

[0031] In the titanyl sulfate deionized water, slowly add 2mol / L potassium carbonate solution, the whole process is controlled to control the reaction temperature not to exceed 40℃, and the pH is 9 to terminate; filter and wash until 0.1mol / L BaCl 2 Solution can not detect SO 4 2- Add 2mol / L hydrochloric acid under stirring conditions to dissolve the resulting filter cake, and control the temperature at 20℃, when it is completely dissolved, stop adding acid; add 10% sodium salicylate, and hydrolyze at 85℃ for 1.5h Afterwards, the product is filtered, washed, dried at 40°C, moved into a muffle furnace and calcined at 630°C for 1.5 hours to obtain mixed crystal titanium dioxide powder with rutile type accounting for 25% and anatase accounting for 75%.

[0032] X-ray diffraction pattern such as figure 1 (d) Shown.

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PUM

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Abstract

The invention relates to a method to make nm titanium dioxide by controlling crystallographic form. The feature includes the following steps: using titanyl sulfate solution as raw material, inorganic base as precipitant to mix and whisk to gain positive titanic acid deposition; filtering the deposition, washing until SO42- can't be detected; adding hydrochloric acid, whisking to resolve the filter cake; adding crystallographic form controlling agent, taking hydrolytic reaction for 0.5-1.5 hour at 85-105 degree centigrade, filtering, washing, and drying at 40-120 degree centigrade, sintering in muffle furnace at 600-700 degree centigrade for 1.5 hour to gain rutile and mixture crystal titanium dioxide of anatase. The invention has great meaning for industrial producing nm titanium dioxide.

Description

Technical field [0001] The invention relates to a method for preparing nano-scale titanium dioxide by controlling crystal form, and belongs to the technical field of chemical synthesis and purification. Background technique [0002] Titanium dioxide has three structures: rutile, anatase and brookite. Among them, brookite is rarely used in industry. Anatase nano-titanium dioxide has stable chemical properties and corrosion resistance. It is an important photocatalytic material. It has great application value in treatment, antibacterial and air purification. Rutile titanium dioxide has high refractive index, excellent light transmittance and strong ultraviolet shielding ability, making it suitable for high-end coatings, cosmetics, polymer materials, and cultural relics protection. There are huge application prospects in such aspects. [0003] The technical route for preparing nano-titanium dioxide can be roughly divided into four types: alkaline hydrolysis and neutralization proces...

Claims

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Application Information

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IPC IPC(8): C01G23/053
Inventor 李志林李强申世刚
Owner HEBEI UNIVERSITY
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