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Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture

A technology of titanium tetrachloride and crude titanium tetrachloride, applied in the direction of titanium halide, etc., can solve the problem of few reports on vanadium removal process, and achieve the effect of low cost

Inactive Publication Date: 2009-10-07
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the crude titanium tetrachloride of low vanadium content (about 0.024wt%), adopt copper method, aluminum method, hydrogen sulfide method and mineral oil etc. to refine existing some reports separately for raw material, but for high vanadium content (about 0.3wt%) ) of crude titanium tetrachloride vanadium removal process reports are still less

Method used

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  • Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture
  • Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture

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Embodiment Construction

[0023] 1. In a rectification column kettle device (see attached figure 1 ), add crude titanium tetrachloride (vanadium content is 0.29wt%) 150g, aluminum powder 0.20g, white oil 0.60g and AlCl 3 0.15 g (average particle size: 200±20 mesh) was mixed, and the mixture was heated to boiling temperature of 138° C. and kept under reflux for 20 minutes. Then raise the temperature to 139-141°C, and collect the distillate whose temperature ranges from 136°C to 137°C at the top of the tower, which is refined titanium tetrachloride. After analysis, the V content of this product was 3 ppm.

[0024] 2. In a rectification column kettle device (see attachedfigure 1 ), add crude titanium tetrachloride (0.29wt% vanadium content) 150g, white oil 1.2g, stir and heat the mixture to boiling temperature 138°C and keep reflux for 100min, observe that there is obvious brown-black precipitate sticking in the tower kettle inner wall of the container. Then raise the temperature to 139-141°C, and coll...

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Abstract

Method of refining titanium tetrachloride by using aluminium powder and vash oil mixture. The method is refining of coarse titanium tetrachloride containing high content of vanadium impurities. Mixing aluminium powder, vash oil and a few AlCl[3] in certain percentage and adding into bottom of fractionating tower containing coarse titanium tetrachloride. Heating the bottom of fractionating tower at a temperature of 139 DEG and regulating reflux ratio of the tower, this moment the aluminium powder and mineral oil deoxidizing the VOCl[3] into lower valency indissoluble precipitate VOCl[2] and being removed, and the TiCl[4] and some low boiling point chemical compounds volatilizing into a reflux unit, extracting cuts of 136-137 DEG boiling point, then condensing to get fine titanium tetrachloride. The vanadium-removed fine titanium tetrachloride contains vanadium content of V%<=0.0007%. The vanadium removing process and the fractionating process are all proceeded in the fractionating tower that saves device. The invention reduces a large amount of residue and sewage discharge, and consumes less materials relative to technics of using aluminium powder and mineral oil to remove vanadium alone, the invention provides high refining efficiency, simple operation and continuous, and has economic and environmental benefit of energy-saving and emission-reduction.

Description

technical field [0001] The invention belongs to the field of rare metal metallurgy and relates to a method for removing crude titanium vanadium tetrachloride impurities by using aluminum powder and mineral white oil as refining reagents. The method is aimed at refining crude titanium tetrachloride with high vanadium impurity content. Background technique [0002] Titanium tetrachloride (TiCl 4 ) is the most important intermediate product in the production of titanium dioxide by the chloride method and the production of sponge titanium by the Krall method. Titanium dioxide (chemical name TiO 2 ) is an important chemical raw material with excellent physical, chemical, optical and pigment properties, and is widely used in industrial fields such as coatings, papermaking, plastics, chemical fibers, rubber, and electrical appliances. In recent years, especially nano-TiO 2 The development of its application has been further expanded, such as for catalysts, cosmetics, food packa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
Inventor 袁章福熊绍锋席亮王晨钰傅振祥战亚鹏
Owner PEKING UNIV
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