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Method for preparing high-purity titanium dioxide by hydrolysis of industrial titanium sulfate solution

A technology for industrial sulfuric acid and titanium dioxide, applied in the directions of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of high impurity content, low product purity, complex process, etc., and achieve the effect of simple process, broad application prospects and low cost.

Active Publication Date: 2022-04-15
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] High-purity titanium dioxide is mostly prepared by direct hydrolysis of titanium tetrachloride, hydrolysis of titanium alkoxide, chloride and sulfuric acid, but the first three processes have problems such as high cost and complicated process.
The preparation of high-purity titanium dioxide by the sulfuric acid method has the advantages of simple and mature process, readily available raw materials, low cost, and simple equipment. However, due to the high impurity content of the preparation system itself and the introduction of other impurities, the product purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The industrial sulfate solution is frozen to 0 to 5 ° C, freezing time 1 h, and the cold freeze-free crystal and solid particles are removed, and the iron sulfate solution after iron is obtained. The 0.58 volume of deionized water was placed in a hydrolyzed pan with heating stirring and condensed reflux, and preheated to 96 ° C. Take 1 volume of sulfuric acid method in the titanium white production process to freeze the iron sulfate solution after iron, preheated to 96 ° C, TiO 2 The concentration was 187 g / L; then stirred, and the preheated titanium liquid was uniformly added to the hydrolysis pot in 20 minutes, and then heated with water to boil in 10 minutes, and the hydrolyzing system was treated with a slightly boiled for 30 minutes, stop heating and stirring. Metprising; after 20 minutes, re-opening heating and heating in 10 minutes to boiling, and maintain a slightly boiling state for 150 minutes, end hydrolysis, to obtain hydrolysis.

[0047] The resulting hydroly...

Embodiment 2

[0049] The industrial sulfate solution is frozen to 0 to 5 ° C, freezing time of 0.8 h, and the cold freeze-free crystal and solid particles are removed, and the iron sulfate solution after iron is obtained. 0.42 volumes of deionized water were placed in a hydrolyzed pan with heating stirring and condensed reflux, and preheated to 94 ° C. Take 1 volume of sulfuric acid method in titanium white production process to preheat the iron sulfate solution after iron, TiO 2The concentration was 173 g / L; then the preheated titanium liquid was uniformly added to the hydrolyzate in 18 minutes, followed by heating the water to boil in 12 minutes, and maintaining the hydrolyzing system for 35 minutes, stopping heating and stirring for ripening; After 25 minutes, the heating stirred and heated in 12 minutes to boiling, and kept the microbeiled state for 180 minutes, end hydrolysis, and hydrolyzed.

[0050] The resulting hydrolyzed gas was cooled to 70 ° C, filtered with filter cake, washed wi...

Embodiment 3

[0052] The industrial sulfate solution is frozen to 0 to 5 ° C, freezing time 0.5 h, and the cooling crystals and solid particles are removed, and the iron sulfate solution after iron is obtained. The 0.35 volume of deionized water was placed in a hydrolyzed pan with heating stirring and condensed reflux, and preheated to 92 ° C. Take 1 volume of sulfuric acid method in titanium white production process to preheat the iron sulfate solution after iron after iron to 92 ° C, TiO 2 The concentration was 165 g / L; then the preheated titanium liquid was uniformly added to the hydrolyzate in 22 minutes, and then heated with water to boil in 15 minutes, and the hydrolyzing system was sealed for 25 minutes, stop heating, and stirring After 27 minutes, re-opening heating and heated to boiling within 10 minutes, and retained a microbeiled state for 180 minutes, end hydrolysis, and hydrolyzed.

[0053] The resulting hydrolyzed material was cooled to 63 ° C, filtered to filter the filter cake...

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PUM

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Abstract

The invention relates to a method for preparing titanium dioxide, in particular to a method for preparing high-purity titanium dioxide by hydrolysis of industrial titanium sulfate solution, which belongs to the technical field of chemical industry. The method for preparing high-purity titanium dioxide by hydrolysis of industrial titanium sulfate solution includes: freezing the titanium sulfate solution to precipitate ferrous sulfate crystals, filtering to obtain filtrate A; taking 1 volume of filtrate A and 0.20-1.00 volume of water and preheating to 90-98 ° C; Then add the filtrate A to the water under stirring conditions, reheat to maintain a slight boiling state for 20-40 minutes, stop heating and stirring and aging for 20-40 minutes; reheat and maintain a slight boiling state for 120-240 minutes, cool to 60-70°C, and Filtrate, wash the filtered solid to obtain purified metatitanic acid; raise the temperature of the purified metatitanic acid to 750-850°C at a rate of 10-15°C / min, keep it warm for 100-150min, and cool to obtain high-purity metatitanic acid Titanium dioxide. The invention directly prepares high-purity titanium dioxide with a purity of more than 99.9% from industrial raw material titanium sulfate, has simple process and low cost.

Description

Technical field [0001] The present invention relates to a method of preparing titanium dioxide, and a method of preparing high purity titanium dioxide, a method of preparing high purity titanium dioxide, comprising a chemical technology. Background technique [0002] Titanium dioxide is stable, as a third largest inorganic chemical, widely used in paints, paints, plastics, paper, chemical fiber, rubber, etc., nearly 90% of titanium resources for the manufacture of titanium white, 2018 my country titanium dioxide Production capacity of 3.55 million tons, production of 2.87 million tons (ranking first in the world), and its annual demand growth is maintained at 2% to 3%. Titanium dioxide also has a semiconductor property, a dielectric constant, and a high-resistance, high-purity titanium dioxide, high-purity titanium dioxide, in such a catalyst carrier, ultraviolet absorber, special glass, electron ceramic, thermistor, semiconductor capacitance, titanic acid. Barium pressure sensit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
Inventor 田从学陈华
Owner PANZHIHUA UNIV