Method for carrying out vanadium removal on coarse titanium tetrachloride

A technology of coarse titanium tetrachloride and titanium tetrachloride, which is applied in the direction of titanium tetrachloride and titanium halide, can solve the problems of aluminum trichloride not up to standard and mildness, and achieve less residue, good settling performance, and Good effect of vanadium

Inactive Publication Date: 2016-12-21
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For crude titanium tetrachloride with high vanadium content, in order to avoid the defect that the aluminum trichloride in the final product does not meet the standard by using the existing aluminum powder vanadium removal technology in the sponge titanium plant, make full use of the existing complete device for aluminum powder vanadium removal , and to overcome the defect of residue sticking to the wall caused by the removal of vanadium by organic matter, the present invention provides a method for removing vanadium by titanium tetrachloride, using the method provided by the invention, the effect of removing vanadium is good, and the conditions are relatively mild

Method used

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Effect test

Embodiment approach

[0029] According to a preferred embodiment of the present invention, the step of removing vanadium from the aluminum powder includes: preparing a titanium trichloride slurry, and performing a second contact with the liquid phase obtained in step (1) with the titanium trichloride slurry.

[0030] Wherein, the preparation process of the titanium trichloride slurry can be a conventional choice in the art, for example, the titanium trichloride slurry can be prepared with aluminum powder and titanium tetrachloride in the presence of aluminum trichloride, or it can be prepared in the general Prepare titanium trichloride slurry with aluminum powder and titanium tetrachloride under the condition of chlorine gas.

[0031] According to a preferred embodiment of the present invention, the present invention uses aluminum powder and titanium tetrachloride to prepare titanium trichloride slurry under the condition of flowing chlorine gas. Specifically, under an inert atmosphere, mix refined...

Embodiment 1

[0042] This embodiment is used to illustrate the method that the crude titanium tetrachloride provided by the present invention removes vanadium

[0043] (1) 500 g of crude titanium tetrachloride having a vanadium content of 0.5% by weight and 15 g of mineral oil were added to a round bottom flask, and stirred at 45° C. for 1 hour. There is no phenomenon of residue sticking to the wall. The mixture in the round-bottomed flask was placed in a 1L measuring cylinder, and was left to settle at 25° C. for 3 hours to obtain 419 g of liquid phase and 94 g of vanadium-containing mud in the lower layer. Then samples were taken at different heights of the liquid phase, and the solid content and vanadium content (measured by taking the supernatant after centrifugation) were carried out by centrifugation. Among them, the maximum solid content of the liquid phase part is 9g / L. After analysis, the vanadium content in the liquid phase was 0.1336% by weight.

[0044] (2) Under the protecti...

Embodiment 2

[0047] This embodiment is used to illustrate the method that the crude titanium tetrachloride provided by the present invention removes vanadium

[0048] (1) 500 g of crude titanium tetrachloride having a vanadium content of 0.5% by weight, 2.5 g of nonanoic acid, and 2.5 g of oleic acid were added to a round bottom flask, and stirred at 80° C. for 0.5 hours. There is no phenomenon of residue sticking to the wall. The mixture in the round-bottomed flask was placed in a 1L measuring cylinder, and was left to settle at 30° C. for 1 hour to obtain 404 g of liquid phase and 97 g of vanadium-containing mud in the lower layer. Then samples were taken at different heights of the liquid phase, and the solid content and vanadium content were determined by centrifugation. Wherein, the maximum solid content of the liquid phase part is 10g / L. After analysis, the vanadium content in the liquid phase was 0.1109% by weight.

[0049] (2) Under the protection of nitrogen, prepare a suspensi...

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Abstract

The invention relates to the field of refining of titanium tetrachloride, and discloses a method for carrying out vanadium removal on coarse titanium tetrachloride. The method comprises: (1) carrying out first contact on coarse titanium tetrachloride with vanadium content of 0.3 weight percent or over 0.3 weight percent and an organic vanadium removal reagent, and carrying out solid-liquid separation on a product obtained by the first contact, wherein the first contact enables vanadium content in a liquid phase obtained by the solid-liquid separation to be reduced to 0.2 weight percent or below 0.2 weight percent; (2) carrying out aluminium powder vanadium removal on the liquid phase obtained by the solid-liquid separation. When the method disclosed by the invention is adopted to process the coarse titanium tetrachloride with high vanadium content, the existing aluminium powder vanadium removal integral device is sufficiently utilized, a small quantity of residues is generated, a vanadium removal effect is good, and generated solid has good settleability.

Description

technical field [0001] The invention relates to the field of refining titanium tetrachloride, in particular to a method for removing vanadium from crude titanium tetrachloride. Background technique [0002] Titanium tetrachloride 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. Crude titanium tetrachloride refers to unpurified titanium tetrachloride, which is a reddish brown or dark yellow turbid liquid, and its color is related to the impurity content in it. The impurity components in crude titanium tetrachloride are very complex, among which vanadium is a main impurity element in crude titanium tetrachloride, which is represented by VOCl 3 form exists in it. VOCl 3 When it is reduced, the oxygen element may enter the sponge titanium at four times the concentration, resulting in an increase in the oxygen content in the sponge titanium, an increase in the Brin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
CPCC01G23/024C01P2006/80
Inventor 周丽李良李冬勤杜明陆平
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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