Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size

A dual-effect seed crystal, high activity technology, used in titanium dioxide, titanium oxide/hydroxide, etc.

Inactive Publication Date: 2014-11-05
SICHUAN LOMON TITANIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many foreign reports on the use of TiCl4 to prepare seed crystals, such as US3560234, US3169074A1, US2571150A1, etc. These patents mainly refer to the preparation method of titanium tetrachloride seed crystals, and also describe the preparation method of titanium tetrachloride Seeds promote the conversion of rutile, but a certain amount of calcined seeds need to be added during calcination, and there is no explanation on how to use titanium tetrachloride seeds to control the particle size of titanium dioxide

Method used

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  • Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size
  • Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size
  • Method of using TiCl4 to prepare high-activity double-effect crystal seed and control titanium dioxide particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Take industrial grade TiCl 4 Solution (TiCl 4 content above 99%), slowly added to water for dilution under the condition of ice-water bath, accompanied by good stirring, it is advisable not to appear white solid phase, and the released HCl gas is absorbed by alkaline liquid. The preparation concentration is 195g / L (with TiO 2 meter) dilution. Take 500ml of diluted solution and add it to 2351ml NaOH dilute solution (NaOH content 65g / L) accompanied by good stirring. The addition should be completed within 15s. Heat the mixed material to 60°C within 60min at a uniform speed and keep it warm for 30min. Immediately add 2811ml of cold water, and cool down to below 40°C through circulating cooling. The cooling time is controlled within 40min. Slowly add dilute lye (NaOH: 65g / L) to adjust the pH to 6.5. Remove more than 80% of the soluble salts by washing, and then dilute the washed seed crystals to 31g / L for later use.

Embodiment 2

[0059] Take industrial grade TiCl 4 Solution (TiCl 4 The content is about 50%), slowly added to water for dilution under the condition of ice water bath, accompanied by good stirring, it is advisable not to appear white solid phase, and the released HCl gas is absorbed by alkaline liquid. The preparation concentration is 205g / L (with TiO 2 count). Take 500ml of diluent and add it to 2213ml NaOH dilute solution (NaOH content 70g / L) with good stirring. The addition should be completed within 15s. Heat the mixed material to 90°C within 60min at a uniform speed and keep it warm for 30min. Immediately add 2811ml of cold water, and cool down to below 40°C through circulating cooling. The cooling time is controlled within 40min. Slowly add dilute lye (NaOH: 70g / L) to adjust the pH to 9.0. Remove more than 80% of the soluble salts by washing, and then dilute the washed seed crystals to 35g / L for later use.

Embodiment 3

[0061] Take industrial grade TiCl 4 Solution (TiCl 4 The content is about 80%), slowly added to water for dilution under the condition of ice-water bath, and accompanied by good stirring, it is advisable not to appear white solid phase, and the released HCl gas is absorbed by alkaline liquid. The preparation concentration is 200g / L (with TiO 2 count). Take 500ml of the above diluted solution and add it into 2311ml NaOH dilute solution (NaOH content 65g / L) with good stirring. The addition should be completed within 15s. Heat the mixed material to 85°C within 60min at a uniform speed and keep it warm for 30min. Immediately add 2811ml of cold water, and cool down to below 40°C through circulating cooling, control the cooling time within 40min, slowly add dilute lye (NaOH: 65g / L) to adjust the pH to 7.0. Remove more than 80% of the soluble salts by washing, and then dilute the washed seed crystals to 33g / L for later use.

[0062]

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Abstract

The invention provides a method of using TiCl4 to prepare a high-activity double-effect crystal seed and control titanium dioxide particle size. Specifically, the method employs TiCl4 as a raw material, a precipitate is prepared through a certain proportion and rapid neutralization of a dilute base solution, the precipitate is subjected to peptizing, curing and quenching and then is adjusted to have a proper pH value, then soluble salt compositions are removed through washing, so that the high-activity double-effect crystal seed, which is applied to hydrolysis process and calcining process of production of sulfuric-acid-process titanium dioxide, is prepared. The prepared crystal seed is uniform in particle size and high in activity, and also during application of hydrolysis of a titanium solution, by adjusting the addition amount of the seed crystal and cooperating with addition of a proper salt treating agent and control on calcining intensity, rutile type titanium dioxide with different particle sizes can be prepared, and thus the particle size demands on different products are satisfied. The preparation technology is simple, not high in equipment investment and high in operation controllability, and the prepared double-effect crystal seed is capable of producing titanium dioxide hydrate primary particles with uniform particle size, so that the uniformity of calcined product particle size is guaranteed, and optical performances and pigment performances of titanium dioxide are perfectly exhibited.

Description

technical field [0001] The invention relates to the technical field of titanium dioxide preparation, in particular to a TiCl 4 A method for preparing a high-activity double-effect seed crystal that can not only promote the progress of hydrolysis, but also promote the transformation of the crystal form during calcination as a raw material and a method for controlling the particle size of titanium dioxide. technical background [0002] In the production of titanium dioxide by sulfuric acid method, the hydrolysis of titanium liquid is one of the four key technologies in the production process of titanium dioxide. The hydrolysis process directly affects the quality of titanium dioxide, so the hydrolysis process has attracted much attention. The hydrolysis process can be divided into two types: autogenous seed crystals and external seed crystals according to the formation method of seed crystals. The essence of both self-generated seed crystals and external seed crystals is the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 周春勇孙润发熊怀忠常建
Owner SICHUAN LOMON TITANIUM IND CO LTD
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