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Method for producing pigment-grade titanium dioxide by circulating hydrochloric acid microemulsion method

A pigment-grade, microemulsion technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of comprehensive recycling and utilization of vanadium-titanium-magnetite resources, environmental pollution of blast furnace slag, and difficulty in realizing industrial production, etc., to achieve The effect of solving the difficulty of comprehensive recycling

Inactive Publication Date: 2017-03-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] In view of the high energy consumption and the difficulty in realizing the technical status quo of industrialized production in the titanium-rich blast furnace slag / ilmenite extraction method of the prior art, the purpose of the present invention is to provide a method that uses titanium-rich blast furnace slag / ilmenite as raw material The method of producing pigment-grade titanium dioxide by circulating hydrochloric acid microemulsion method to solve the environmental pollution of blast furnace slag and the difficulty of comprehensive recovery and utilization of vanadium-titanium-magnetite resources

Method used

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  • Method for producing pigment-grade titanium dioxide by circulating hydrochloric acid microemulsion method
  • Method for producing pigment-grade titanium dioxide by circulating hydrochloric acid microemulsion method
  • Method for producing pigment-grade titanium dioxide by circulating hydrochloric acid microemulsion method

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Embodiment 1

[0034] The process of this embodiment is attached figure 1 Shown, is the use of titanium-rich blast furnace slag to produce rutile titanium dioxide and other resources in the recovery of raw materials.

[0035] (1) TiO 2 100 parts by mass of blast furnace slag with a mass content of 25% (generally 20-42%), ground and sieved to 200 mesh, added to the hydrolysis reactor for acid hydrolysis, and the mass concentration of hydrochloric acid in the acid hydrolysis process is controlled to be about 20% (generally controlled in the range of 15-34%), the amount of hydrochloric acid is added according to the liquid-solid mass ratio of 4:1 (the liquid-solid ratio is generally controlled in the range of 4-8:1), and the temperature is about 85°C (generally controlled in 80-105 ℃ range), the time is about 120min. The acid hydrolyzed slurry is filtered and washed, and the obtained acid hydrolyzed clear liquid enters the next process, and the obtained silicon residue can be used as a high-s...

Embodiment 2

[0048] The process of this embodiment is attached figure 2 Shown, is the use of titanium-rich blast furnace slag to produce nano-scale or sub-nano-scale rutile titanium dioxide and other resources in the recovery of raw materials.

[0049] In the flow process of this embodiment, except that the treatment process of the organic extract discharged from the No. 1 extractor is different from the flow process in Example 1, the flow process of other parts is the same as the flow process in Example 1. In this example, the organic microemulsion added to the No. 1 extractor needs to be swollen with water and a small amount of lye before it is added to the No. 1 extractor, so that it forms an inner phase coated with an alkaline liquid. The temperature of the organic extract discharged from the No. 1 extractor is raised to 70-80°C to disintegrate the inner phase of the microemulsion to a certain extent, and then it is sent to a high-speed centrifuge to hydrolyze the microbubbles. The h...

Embodiment 3

[0055] The process of this embodiment is attached image 3 As shown, it is to use refractory vanadium-titanium magnetite or titanium concentrate to directly produce rutile titanium dioxide and recover other resources in raw materials.

[0056] The flow process of this embodiment is different from the process flow of Example 1. One is that the acidolysis slurry discharged from the acidolysis reactor is filtered and washed to obtain the acidolysis clear liquid. (generally controlled at -10-5°C) crystallization reaction for about 120 minutes (generally controlled in the range of 60-180 minutes), so that the ferric chloride and ferric chloride contained in it are crystallized and separated by a centrifuge to obtain ferric chloride And the preliminary purified acid hydrolysis clear liquid, in which ferric chloride can be decomposed by spraying to obtain high-grade ferric oxide, that is, iron concentrate; to obtain iron red, it is only necessary to separate and purify the liquid bef...

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Abstract

The invention discloses a preparation method of pigment-level titanium dioxide powder by a cyclic hydrochloric acid micro emulsion method. The preparation method mainly comprises the following steps of: carrying out acidolysis on titanium-enriched blast furnace slag or ilmenite by utilizing hydrochloric acid to obtain a clear acidolysis liquid; extracting titanium with an organic micro emulsion; collecting titanium in the clear acidolysis liquid by superfine liquid ball formed by a micro emulsion film in the organic micro emulsion; separating organic micro emulsion into organic extract liquor and raffinate; carrying out reextraction on the obtained organic extract liquor with reextraction agent to remove titanium; and hydrolyzing and calcining the obtained reextraction titanium liquid to obtain rutile type titanium dioxide, extracting and removing the impurities, such as iron, aluminum, magnesium and vanadium, in the raffinate by the organic micro emulsion, and returning obtained regenerated hydrochloric acid back to the acidolysis process. By using the method of the invention, the problems that the preparation method of the titanium dioxide powder in the prior art is high in vitriol cycle energy consumption and industrialization is hard to realize can be overcome, various byproducts can be prepared while the titanium dioxide powder is prepared, and resources in raw materials can be comprehensively recycled, so that the pollution problem of blast furnace slag on environment can be basically solved.

Description

technical field [0001] The invention relates to a production method of titanium dioxide, in particular to a method for producing pigment-grade titanium dioxide by using titanium-rich blast furnace slag / ilmenite as raw material and adopting a circulating hydrochloric acid microemulsion method. It belongs to the field of comprehensive utilization of resources and environmental protection. Background technique [0002] Titanium is one of the important strategic resources that all countries in the world attach great importance to. China's titanium resources mainly come from vanadium-titanium magnetite, accounting for about 86% of the country's total reserves, mainly concentrated in Panzhihua, Sichuan. At present, the utilization rate of titanium in China's vanadium-titanium magnetite is only 10-16%, most of which are enriched in blast furnace slag and discharged after blast furnace smelting. Blast furnace slag generally contains TiO 2 About 20-25wt%, also contains silicon, ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/08
Inventor 刘代俊毛雪华张鹏张建钧
Owner SICHUAN UNIV
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