Method for preparing rutile-type titanium dioxide

A titanium dioxide and rutile-type technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve problems such as complex process flow, achieve simple process flow, simplify process flow, and reduce raw material costs

Inactive Publication Date: 2013-08-28
河北中科同创科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dilute titanium liquid TiO after separation of ferrous iron by freezing and crystallization in sulfuric acid process 2 The concentration is generally about 150g / L. In order to prepare qualified pigment-grade titanium dioxide, the dilute titanium solution must be concentrated in vacuum until it is concentrated to TiO2. 2 200±5g / L (for pressurized hydrolysis) or TiO 2 215~230g / L (for normal pressure hydrolysis), resulting in complex process; in addition, when producing rutile titanium dioxide, it is necessary to add a large amount of rutile calcined seeds and carry out long-term high-temperature calcination (>950°C)

Method used

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  • Method for preparing rutile-type titanium dioxide

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The titanium slag (TiO 2 The mass content is 49.0%), mixed evenly under stirring, and reacted at 150°C for 2.5h, wherein, the solid-liquid mass ratio of acid-leached titanium slag and sulfuric acid was 1.5:1, and the intermediate product obtained after the reaction was mixed with 5% The dilute sulfuric acid for three-stage countercurrent leaching, wherein the mass ratio of the intermediate product to dilute sulfuric acid for leaching is 1:1.2. After filtering, add the ammoniacal liquor that mass percentage concentration is 25% in gained filtrate, wherein ammoniacal liquor addition is 22% of filtrate volume, then add trivalent titanium solution as reductant, make ferric iron all be reduced to ferrous iron, obtain TiO 2 The concentration is 108g / L titanium liquid, and finally hydrolysis is carried out at 120°C for 3 hours, and the hydrolyzed product is filtered to obtain a white hydrated titanium dioxide solid, which is calcined at 850°C for 2 hours to obtain rutile tita...

Embodiment 2

[0034] The titanium slag (TiO 2 The mass content is 52.4%), mixed evenly under stirring, and reacted at 200°C for 0.5h. The dilute sulfuric acid for three-stage countercurrent leaching, wherein the mass ratio of the intermediate product to dilute sulfuric acid for leaching is 1:1.5. After filtering, add 25% ammonia water to the obtained filtrate, wherein the amount of ammonia water added is 12% of the volume of the filtrate, and then add iron powder as a reducing agent to reduce all ferric iron to ferrous iron to obtain TiO 2The concentration is 120g / L titanium liquid, and finally hydrolysis is carried out at 115°C for 3.5 hours, and the hydrolyzed product is filtered to obtain a white hydrated titanium dioxide solid, which is calcined at 900°C for 2 hours to obtain rutile titanium dioxide; the hydrolyzed mother liquor is slowly heated at 85°C for 4 Hour, wherein, the solid-liquid mass ratio of vitriol and hydrolysis mother liquor is 1:35, obtains light green ferrous ammonium...

Embodiment 3

[0036] The sulfuric acid solution obtained in Example 2 (mass percentage concentration is 85%) is circulated back to the sulfuric acid solution of the reactor and the titanium slag (TiO 2 The mass content is 49.8%), mixed evenly under stirring, and reacted at 180°C for 1h, wherein the solid-liquid mass ratio of acid-leached titanium slag and sulfuric acid was 1.3:1, and the intermediate product obtained after the reaction was mixed with 20% Dilute sulfuric acid is used for three-stage countercurrent leaching, wherein the mass ratio of intermediate product to dilute sulfuric acid for leaching is 1:0.8. After filtering, add 28% ammoniacal liquor to the obtained filtrate, wherein the amount of ammoniacal liquor added is 7% of the volume of the filtrate, and then add sodium sulfite as a reducing agent to completely reduce ferric iron to ferrous iron to obtain TiO 2 The concentration is 125g / L titanium liquid, and finally hydrolysis is carried out at 80°C for 8 hours, and the hydro...

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Abstract

The invention belongs to the field of preparation of inorganic metal compounds, and particularly relates to a method for preparing rutile-type titanium dioxide. The method for preparing rutile-type titanium dioxide comprises the following steps: 1) adding sulfuric acid into titanium slag to obtain an acid hydrolysate; 2) leaching the acid hydrolysate obtained in the step 1) with dilute sulfuric acid; 3) filtering the titanium solution obtained in the step 2), adding ammonia water into the obtained filtrate, and adding a reducer to obtain a titanium solution in which the TiO2 concentration is 100-130 g/L; 4) hydrolyzing the titanium solution obtained in the step 3), and filtering to obtain a titanium dioxide hydrate solid and a hydrolysis mother solution; and 5) calcining the titanium dioxide hydrate obtained in the step 4) to obtain the rutile-type titanium dioxide. The invention provides a clean production method for producing rutile-type titanium dioxide from low-grade titanium slag, and provides an effective way for comprehensively utilizing titanium resources and preparing titanium dioxide (titanium white).

Description

technical field [0001] The invention belongs to the field of preparation of inorganic metal compounds, in particular, the invention relates to a method for preparing rutile titanium dioxide. Background technique [0002] Titanium dioxide, commonly known as titanium dioxide, is currently the most widely used white pigment, accounting for 80% of all white pigments used. It is also the most important product of the titanium series. 90% of the world's total titanium resources are used to manufacture titanium dioxide. Titanium dioxide is widely used in many fields such as modern industry and agriculture, national defense, science and technology, and has a close relationship with people's lives and the national economy. contact. [0003] Compared with anatase titanium dioxide, rutile titanium dioxide has higher hiding power, light loss resistance and chalking resistance, not only has stable physical and chemical properties, but also has excellent optical and electrical properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 齐涛赵龙胜刘亚辉王丽娜陈德胜赵宏欣仲斌年胡国平
Owner 河北中科同创科技发展有限公司
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