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Method of removing vanadium from titanium tetrachloride by aluminum powder as direct reducer

A technology of titanium tetrachloride and reducing agent, applied in titanium halide and other directions, can solve problems such as troublesome and difficult transportation and measurement

Inactive Publication Date: 2007-03-14
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many disadvantages in this "two-step method": (1) the production of TiCl 3 The slurry needs to add AlCl 3 Or first react with chlorine and aluminum powder to generate AlCl 3 As a catalyst; (2) TiCl that needs to be manufactured 3 The slurry is sent to the vanadium removal reactor where TiCl is present 3 Trouble and difficulty in slurry manufacturing, transportation and metering; (3) Although the vanadium removal process can achieve continuous operation, TiCl 3 Slurry manufacturing is a batch process

Method used

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  • Method of removing vanadium from titanium tetrachloride by aluminum powder as direct reducer

Examples

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Effect test

Embodiment 1

[0028]Add 5kg of spherical aluminum powder with an average particle diameter of 80 μm into a closed surface activation processor, add 0.2 kg of stearic acid, and mechanically grind for 6 hours under the protection of an argon atmosphere to obtain 5.2 kg of flake aluminum powder with an average particle diameter of 40 μm, wherein Contains 3.6% surfactant

Embodiment 2

[0030] In a reactor with a condensing reflux device, titanium tetrachloride containing vanadium impurities (where VOCl 3 0.10%) 500g, anhydrous AlCl 3 3 g and 250 mg of surface-activated aluminum powder (average particle size 40 μm) were mixed, the mixture was heated to boiling (137° C. to 138° C.), and kept in a boiling reflux state for 30 minutes. After the vanadium removal reaction was completed, the reaction mixture was settled and cooled to 0°C, and the upper clear liquid 250ml and the underflow (containing AlCl 3 and VOCl 2 ) 40ml, after analysis the supernatant liquid V content is 3ppm.

Embodiment 3

[0032] In a reactor with a condensing reflux device, titanium tetrachloride containing vanadium impurities (where VOCl 3 0.10%) 500g, 40ml of underflow separated in Example 2 and 100mg of surface-activated aluminum powder (average particle diameter 40 μm) were mixed, and the mixture was heated to boiling (137°C-139°C), and kept in a boiling reflux state for 30 minutes. After the vanadium removal reaction was completed, the reaction mixture was settled and cooled to 0°C, and the upper clear liquid 280ml and the underflow (containing AlCl 3 and VOCl 2 ) 50ml, after analysis the supernatant liquid V content is 3.5ppm.

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Abstract

The process of eliminating vanadium impurity from titanium tetrachloride (TiCl4) product with aluminum powder as direct reductant includes the following steps: feeding TiCl4 solution to be refined and surface activated aluminum powder into rectification tower, adding AlCl3 as catalyst and heating to boiling point to produce vanadium eliminating reaction; evaporating TiCl4 containing AlCl3 and high boiling point impurity inside the rectification tower to eliminate AlCl3 and high boiling point impurity, and condensing TiCl4 vapor escaping through the tower top to obtain refined TiCl4 product; and exhausting tower solution regularly or continuously to maintain the required AlCl3 concentration inside the tower. The said process can eliminate vanadium and high boiling point impurity simultaneously, and has continuous operation, low cost, high product quality and other advantages.

Description

technical field [0001] The invention relates to a method for removing vanadium impurities in titanium tetrachloride, in particular to a method for removing vanadium oxychloride impurities in titanium tetrachloride by using aluminum powder as a direct reducing agent. Background technique [0002] Titanium tetrachloride is the raw material for the production of sponge titanium by the Krall method and the production of titanium dioxide by the chloride method. There are many harmful impurities in the crude titanium tetrachloride produced by chlorination of titanium-containing raw materials. These impurities directly affect the quality of sponge titanium and titanium dioxide. Therefore, crude titanium tetrachloride must be purified before it can be used to produce sponge titanium and titanium dioxide. Titanium dioxide. Most of the impurities in the crude titanium tetrachloride can be separated and removed by sedimentation filtration, distillation and rectification, but the vanad...

Claims

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Application Information

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IPC IPC(8): C01G23/02
Inventor 邓国珠刘水根
Owner GRIMAT ENG INST CO LTD
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