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A kind of preparation method of conductive titanium dioxide powder

A conductive titanium dioxide, titanium dioxide technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of poor weather resistance and gloss, poor repeatability of titanium dioxide method, high cost per unit mass of product, and achieve good dispersion. , Controllable stoichiometric ratio, excellent whiteness and conductivity

Active Publication Date: 2017-08-04
中信钛业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Antimony-doped tin dioxide has excellent electrical conductivity, but the whiteness of the powder is very low, which seriously affects its application range
EP0267535 discloses a method for preparing conductive titanium dioxide, which uses a certain proportion of titanium dioxide and sodium chloride, sodium hydrogen phosphate, zinc oxide, potassium oxide or phosphorus pentoxide to treat it for a period of time at a high temperature of 900 ° C, and then After alkali treatment, acid treatment, and then surface coating, this method has many steps, and the calcining step consumes too much energy and consumes a lot of equipment.
CN102583524A discloses a preparation method of conductive powder coated titanium dioxide with tin oxide containing antimony oxide. The method first uses titanium salt as a titanium source to prepare titanium dioxide, then adds hydrolyzable tin salt and antimony salt, and deposits under controlled conditions Coated, finally dried and calcined, this method has too many steps, and the method of preparing titanium dioxide is not repeatable
CN103985430A discloses a method for preparing conductive titanium dioxide. In this method, a conductive layer of doped tin oxide is evenly deposited on the surface of titanium dioxide particles, but the concentration of the titanium dioxide suspension prepared by this method is as low as 10-20%. High cost per unit mass product
The conductive titanium dioxide prepared by the above method has a common defect, that is, the weather resistance and gloss of the product are not as good as the usual pigment grade titanium dioxide in the fields of coatings, plastics and fibers.

Method used

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  • A kind of preparation method of conductive titanium dioxide powder
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  • A kind of preparation method of conductive titanium dioxide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation method of the conductive titanium dioxide powder, the steps are as follows:

[0029] 1. Beat the rutile titanium dioxide produced by the chlorination method in distilled water, stir it evenly to obtain a slurry with a mass concentration of 20%, take 100ml, and add zirconium sulfate solution dropwise to the obtained slurry, wherein the mass of zirconium sulfate and titanium dioxide Than ZrO 2 / TiO 2 Calculated as 0.1%, the concentration of zirconium sulfate solution is ZrO 2 Count as 120g / L, obtain mixed solution A;

[0030] 2. Drop the mixed acid solution of tin sulfate and antimony trichloride prepared in advance into the mixed solution A at the same time, control the reaction pH=1, the reaction temperature is 60°C, the titration time is 3h, and the alkali solution is oxidized with hydrogen Sodium solution with a concentration of 6mol / L, wherein the concentration of hydrochloric acid in the mixed acidic solution is 20%, and the mass of tin sulfate is...

Embodiment 2

[0033] The preparation method of the conductive titanium dioxide powder, the steps are as follows:

[0034] 1. Beat the rutile titanium dioxide produced by the chlorination method in distilled water, stir evenly to obtain a slurry with a mass concentration of 25%, take 100ml, and add zirconium nitrate solution dropwise to the obtained slurry, wherein the mass of zirconium nitrate and titanium dioxide Than ZrO 2 / TiO 2 Calculated as 0.3%, the concentration of zirconium nitrate solution is ZrO 2 Count as 150g / L, obtain mixed solution A;

[0035]2. Drop the pre-prepared mixed acid solution of tin nitrate and antimony trichloride and potassium hydroxide solution into the mixed solution A at the same time, control the reaction pH=2, the reaction temperature is 70°C, and the titration time is 4 hours. The concentration is 8mol / L, wherein the concentration of hydrochloric acid in the mixed solution is 25%, and the mass of tin nitrate is based on SnO 2 / TiO 2 Calculated as 25%, t...

Embodiment 3

[0040] The preparation method of the conductive titanium dioxide powder, the steps are as follows:

[0041] 1. Beat the rutile titanium dioxide produced by the chlorination method in distilled water, stir evenly to obtain a slurry with a mass concentration of 30%, take 100ml, add zirconium chloride solution dropwise to the obtained slurry, wherein zirconium chloride and titanium dioxide The mass ratio of ZrO 2 / TiO 2 Calculated as 0.5%, the concentration of zirconium chloride solution is ZrO 2 Count as 180g / L, obtain mixed solution A;

[0042] 2. Drop the pre-prepared tin salt and antimony salt mixed acidic solution and alkaline solution into the mixed solution A at the same time, control the reaction pH=3, the reaction temperature is 80°C, the titration time is 5 hours, and the concentration of the ammonia solution is 10mol / L. Wherein the concentration of hydrochloric acid in the mixed solution is 30%, the quality of tin tetrachloride is by SnO 2 / TiO 2 Calculated as 30%...

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Abstract

A method for preparing conductive titanium dioxide powder, the preparation process of which is as follows: 1) adding rutile titanium dioxide into distilled water for beating to form a slurry with a titanium dioxide mass concentration of 20% to 30%, stirring evenly to obtain the titanium dioxide slurry, and then feeding Add the zirconium salt solution dropwise to the titanium dioxide slurry to obtain a mixed solution A; 2) raise the temperature of the mixed solution A to 60-80° C.; 3) add a certain amount of mixed acidic solution of tin salt and antimony salt to the mixed solution In solution A, add lye at the same time to control the pH value from 1 to 3, and the addition time is 3 to 5 hours to obtain a yellow suspension; 4) ripen, wash, and dry the suspension, crush it to 280 to 300 nm, and then After calcination treatment, the conductive titanium dioxide powder can be obtained. The conductive titanium dioxide prepared by this method has excellent properties such as electrical conductivity, whiteness, hiding power, weather resistance and gloss when applied in coatings, plastics, fibers and other application fields, and is a new material with broad application prospects.

Description

technical field [0001] The invention relates to a preparation method of conductive titanium dioxide powder. Background technique [0002] Antimony doped tin oxide (ATO for short) is an n-type semiconductor material. dispersion , resistance to activity, Thermoplastic , wear resistance , There are other conductive materials (such as graphite , surfactants, metal powders, etc.) have incomparable advantages. Its powder has excellent electrical conductivity, and its loose density is smaller than that of metal powder. It is stably dispersed in the matrix material and is not easy to aggregate and settle. There will be no decrease in electrical conductivity due to the oxidation of metal powder. Coatings, conductive plastics, infrared absorbing materials and some antistatic materials have broad application prospects, and are a multifunctional material with great development potential. However, the ATO powder after high-temperature sintering is blue-green powder, and my countr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047
Inventor 齐牧姜志刚马恩泉王建伟张贺任健
Owner 中信钛业股份有限公司
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