Hydrogen sulfide vanadium removal technology

Abstract

The invention provides a hydrogen sulfide vanadium removal technology which comprises the following steps: injecting coarse TiCl4 into a reaction kettle A; directly introducing hydrogen sulfide gas and nitrogen into the reaction kettle A, wherein the mass ratio of the hydrogen sulfide gas to the coarse titanium tetrachloride is (1-2):1,000; controlling the temperature in a reaction kettle B to 120-130 DEG C, and performing an aging reaction for 1-2 hours; and feeding pure titanium tetrachloride to the tower bottom and discharging into a finished product tower kettle to obtain a finished product of TiCl4, wherein the finished product of TiCl4 is colorless and transparent in a liquid form without obvious scaling phenomenon, and the vanadium content in the finished product of TiCl4 is less than or equal to 0.0024%. In the invention, hydrogen sulfide reacts with VOCl3 and impurities in the coarse TiCl4 to generate VOCl2 which is discharged in a form of slurry; and the technological method is simplified, the process is shortened, and the equipment and raw material cost is lowered.

Description

technical field [0001] The invention relates to a process for removing vanadium by hydrogen sulfide, which can be used in the field of vanadium removal by refining titanium tetrachloride. Background technique [0002] Titanium tetrachloride is an important intermediate in the production of titanium metal and its compounds, and is the main raw material for the production of titanium sponge and titanium dioxide by chloride process, and its application fields are relatively wide. Crude titanium tetrachloride contains a variety of organic impurities such as vanadium. It needs to be refined before it can be used as a raw material or preparation in the production field. [0003] At present, there are mainly copper wire vanadium removal method, aluminum powder vanadium removal method, mineral oil vanadium removal and other processes. The mechanism is mainly to remove vanadium from crude titanium tetrachloride and reduce VOC1 3 , producing insoluble VOC1 2 , and then use precipita...

AI Technical Summary

Problems solved by technology

Copper wire has a good vanadium removal effect, and can remove impurities such as organic matter at the same time. Copper will not pollute the product, but the problem is that expensive metal copper is consumed, the cost of vanadium removal is high, and the regeneration and cleaning of invalid copper wire balls is labor-intensive. Produce a large amount of acid mist and waste acid water containing copper to pollute the environment

[0004] For mineral oil vanadium removal, a small amount of organic matter is added to the crude TiC1 solution, stirred and heated. If no stirring is added, it is not conducive to the reaction. Stirring can increase the contact between the organic matter and the feed liquid, so that it can fully mix with VOC1 3 The organic matter used in the method of removing vanadium by contact is cheap and non-toxic, which reduces environmental pollution and removes metal impurities such as vanadium. However, the amount of residue after vanadium removal is relatively large, which is easy to scar on the container wall and seriously affects heat transfer.

[0005] CN201010561179.X discloses a method for removing vanadium from titanium tetrachloride, the crude TiCl 4 and AlCl 3 in AlCl 3 The mixed solution is mixed in the preparation tank, and the crude TiCl 4 A series of aluminum powder vanadium removal processes such as mixing with aluminum powder in the aluminum powder mixture preparation tank still have the problems of complicated processes such as filtration, evaporation heat exchange, and fine distillation, the amount of residue is relatively large, and the vanadium removal effect is not ideal

[0006] There are many and complex vanadium removal processes in the refining of titanium tetrachloride, which not only exist in copper wire vanadium removal method and aluminum powder vanadium removal method, but also in mineral oil vanadium removal process, which requires continuous stirring and heating treatment, and the condenser and pipeline will be generated during cooling. Blockage, more mud will be generated and the recovery rate of titanium tetrachloride will be reduced. It needs to go through the three-tower refining and vanadium removal process. The first tower removes vanadium, the second tower removes silicon tetrachloride, and the third tower removes hydrocarbons, etc.; and other Some vanadium removal processes remove impurities in titanium tetrachloride, the amount of residue is relatively large, and it is easy to corrode the container equipment, and the solid-liquid ratio of titanium tetrachloride after the organic vanadium removal reaction is high, and it is easy to block the pipeline. Therefore, for titanium tetrachloride The vanadium removal effect of the refining process is not ideal and needs to be improved

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