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A method for preparing high-purity titanium dioxide from titanium-containing blast furnace slag

A technology of titanium dioxide and blast furnace slag, applied in the direction of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., can solve the problems of high impurity content, low titanium concentration, low yield, etc., to improve acidolysis conversion rate, The effect of reducing the amount of sulfuric acid and promoting hydrolysis

Active Publication Date: 2021-11-23
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with the industrial titanyl sulfate solution, the heterogeneous titanyl sulfate solution obtained by this method has a low titanium concentration (Ti concentration (in terms of TiO 2 Total) 4 ):>20g / L, c(Al 2 (SO 4 ) 3 ):>20g / L), limited by normal pressure hydrolysis conditions, the titanium liquid needs to be purified and concentrated before the normal pressure self-generation / additional seed crystal hydrolysis operation, there are problems such as long process, large energy consumption, low yield, etc. make its practical application limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Crush and grind titanium-containing blast furnace slag, and sieve through 200 mesh to remove the coarse slag on the sieve; mix the sieved titanium-containing blast furnace slag, sodium dodecylsulfonate, ammonium sulfate and 95% sulfuric acid solution, and the mass ratio of each substance Titanium-containing blast furnace slag: sodium dodecylsulfonate: ammonium sulfate: 95% sulfuric acid solution = 100:0.01:0.1:170, reacted at 80°C, normal pressure, and uniform mixing conditions for 2 hours to obtain the acid hydrolysis product; Mix the acid hydrolysis product with water at a mass ratio of 1:1.5, react at 75°C for 2 hours under uniform stirring conditions, and then filter to obtain a solution containing titanyl sulfate; mix the solution containing titanyl sulfate, sodium sulfate and dodecyl Potassium aluminum sulfate hydrate is mixed according to the mass ratio of 100:0.1:0.01, the mixed solution is placed in a hydrothermal kettle and sealed, and the hydrothermal reaction...

Embodiment 2

[0038] Crush and grind titanium-containing blast furnace slag, and sieve through 400 meshes to remove the coarse slag on the sieve; mix the sieved titanium-containing blast furnace slag, sodium dodecylbenzenesulfonate, ammonium chloride and 85% sulfuric acid, and the mass of each substance The ratio is titanium-containing blast furnace slag: sodium dodecylsulfonate: ammonium chloride: 85% sulfuric acid = 100: 0.05: 0.5: 200, reacted for 3 hours at 120 ° C, normal pressure, and uniform mixing conditions to obtain the acid hydrolysis product Mix the acid hydrolysis product with water at a mass ratio of 1:2.5, react at 60°C for 3 hours under uniform stirring, and then filter to obtain a solution containing titanyl sulfate; mix titanyl sulfate solution, potassium sulfate and aluminum Sodium acid is mixed according to the mass ratio of 100:0.5:0.1, the mixed solution is placed in a hydrothermal kettle and sealed, and the hydrothermal reaction is carried out at 150°C, the pressure is...

Embodiment 3

[0040] Crush and grind titanium-containing blast furnace slag, and sieve through 350 mesh to remove the coarse slag on the sieve; after screening, titanium-containing blast furnace slag, sodium cetyl sulfonate, sodium cetylbenzene sulfonate, ethylenediaminetetra Acetic acid and 90% sulfuric acid are mixed, and each substance mass ratio is titanium-containing blast furnace slag: sodium cetyl sulfonate: sodium cetylbenzene sulfonate: 90% sulfuric acid=100: 0.1: 1: 180, at 100 ℃, React for 0.5 hours under normal pressure and uniform mixing conditions to obtain the acid hydrolysis product; mix the acid hydrolysis product and water at a mass ratio of 1:2.5, react at 75°C for 2 hours under uniform stirring conditions, and then filter to obtain the sulfuric acid containing oxygen Titanium solution: Mix the heterotitanyl sulfate solution, sodium sulfate, ammonium sulfate, and polyaluminium chloride at a mass ratio of 100:0.2:0.4:0.06, place the mixed solution in a hydrothermal kettle a...

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Abstract

A method for preparing high-purity titanium dioxide from titanium-containing blast furnace slag belongs to the technical field of chemical material preparation. The present invention uses titanium-containing blast furnace slag as a raw material, and first obtains a titanyl sulfate solution containing heterogeneous sulfuric acid through a sulfuric acid-enhanced acid hydrolysis method; then uses a selective hydrothermal deposition method to separate impurities and titanium-containing components to prepare a metatitanic acid precursor; The acid precursor is calcined, and the crystal form of the product is controlled by controlling the calcining temperature to obtain anatase-type or rutile-type high-purity titanium dioxide with a purity ≥ 98%, and the total yield of titanium dioxide is ≥ 85%. The main feature of this method is that it uses enhanced acid hydrolysis and selective hydrothermal precipitation to achieve high-efficiency conversion and comprehensive removal of low-grade titanium-containing blast furnace slag, and has the advantages of short process flow, high product purity, high titanium yield, and low acid consumption. The outstanding features provide a new way for the industrial application of titanium-containing blast furnace slag.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, and in particular relates to a method for preparing high-purity titanium dioxide by using titanium-containing blast furnace slag as a raw material. Background technique [0002] Titanium-containing blast furnace slag is a by-product produced in the blast furnace smelting process of vanadium-titanium magnetite, and the mass fraction of each component in the slag is TiO 2 : 21~25%; SiO 2 : 22~26%; CaO: 22~29%; Al 2 o 3 Fe: 16-19%; MgO: 7-9%; total Fe: 0.2-0.4%. At present, the comprehensive utilization rate of titanium-containing blast furnace slag resources is low, and it is mainly used to prepare low-end building materials such as slag cement, sanitary porcelain plates and alkali-resistant mineral wool (Liu Shuai, research status and development prospects of titanium extraction technology from high-titanium blast furnace slag, China Metallurgy, 2020, 30(3), 1~7), but the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
CPCC01G23/0532C01P2006/80
Inventor 向兰王明亮杨卓颖杨帆
Owner TSINGHUA UNIV
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