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Method for comprehensively recycling titanium and niobium from crude titanium tetrachloride precipitate mud

A technology of crude titanium tetrachloride and precipitation mud, which is applied in the fields of comprehensive utilization of resources and chemical separation, can solve the problems of neglecting niobium separation and recovery, difficulty of molten salt regeneration, affecting normal production, etc., and achieves low comprehensive recovery cost, light specific gravity, Easy-to-operate effects

Inactive Publication Date: 2014-01-29
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Returning the sedimentation mud to the fluidized chlorination furnace will cause large fluctuations in furnace conditions and affect normal production; when the sedimentation mud is directly added to the clapboard dust collector, due to the small contact surface between the furnace gas and the mud and the short contact time, the TiCl 4 If it is too late to evaporate, it will accumulate at the bottom of the dust collector; centrifugal drying cannot avoid TiCl 4 Hydrolysis; microwave drying can avoid TiCl 4 Hydrolysis, but the penetration of microwaves in sedimentation mud is limited, it is difficult to be used in industrial production; spray drying can better recover TiCl in sedimentation mud 4 , but the drying process produces a large amount of waste gas; molten salt drying can also better recover TiCl in the sedimentation mud 4 , but the regeneration of molten salt after drying is difficult
The drying methods of the above-mentioned sedimentation mud only care about TiCl 4 The recovery of niobium, while ignoring the separation and recovery of niobium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] TiCl 4 63.5wt% chlorination furnace thickener precipitation mud 50ml, add 1000ml mixed organic solvent composed of benzene and toluene in a volume ratio of 1:1, stir at room temperature for 0.5h, and centrifuge to obtain TiCl-containing 4 4 . The filter residue obtained by centrifugation was first added with water and stirred at a liquid-solid mass ratio of 8:1, then added ammonia water to adjust the pH value of the solution to 0.5, stirred at 50°C for 2 hours, and filtered to obtain 2 o 5 42.6% niobium-containing filter cake.

Embodiment 2

[0020] According to the volume ratio of 1:1, containing TiCl 4 CH 2 Cl 2 , after stirring evenly, settle naturally for 2 hours, pour out the supernatant, and add CH to the bottom sludge at a volume ratio of 1:0.5 2 Cl 2 , stirred at room temperature for 0.5h, and filtered under pressure to obtain TiCl-containing 4 4 . The decanted supernatant was distilled under reduced pressure at 40°C for 10 hours, and the distillate was condensed to obtain CH 2 Cl 2 Recycling, the distillation residue is crude TiCl 4 , into the titanium tetrachloride refining process to separate the impurities. Add water to the filter residue and stir at a liquid-solid mass ratio of 4:1, add lime to adjust the pH value to 0.6, stir at room temperature for 3 hours to separate niobium from impurities such as titanium, aluminum, iron, and calcium, and filter to obtain Nb-containing 2 o 5 35.3% niobium-containing filter cake.

Embodiment 3

[0022] will contain TiCl 4 Add 200ml of 58.2wt% crude titanium tetrachloride precipitation slurry into 450ml of dichloroethane, stir at room temperature for 10min, and vacuum filter to obtain filter residue and filtrate. The filtrate was distilled at 80°C for 2 hours, the distillate was condensed and recycled, and the residue obtained by distillation was crude TiCl 4 . The filter residue was rinsed and drained with 50ml of dichloroethane first, then water was added to stir according to the mass ratio of liquid to solid ratio of 2:1, and then NaOH was added to adjust the pH value to 0.1, stirred at 90°C for 2 hours, and the filter cake obtained by pressure filtration was dried. Contains Nb 2 o 5 52.3%.

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Abstract

The invention discloses a method for comprehensively recycling titanium and niobium from crude titanium tetrachloride precipitate mud, which comprises the following steps: evenly mixing precipitate mud and an organic solvent, carrying out liquid-solid separation, separating the filtrate to recycle the organic solvent and crude TiCl4, separating the filter residue to enrich niobium, and the like. The technical method is simple and convenient to operate, and can recycle TiCl4 entrapped in the crude titanium tetrachloride precipitate mud as well as Nb in the crude titanium tetrachloride precipitate mud; the recovery rates of titanium and niobium are high, the technical process is simple and easy to operate, the organic solvent can be recycled, and the comprehensive recycling cost of titanium and niobium is low; and thus, the invention is suitable for industrialized application.

Description

technical field [0001] The invention relates to a method for comprehensively recovering titanium and niobium from crude titanium tetrachloride precipitation mud; it belongs to the technical field of resource comprehensive utilization and chemical separation. Background technique [0002] Titanium tetrachloride production process, crude TiCl obtained by condensation of chlorination furnace gas 4 The sedimentation slurry separated from the liquid contains 50~60wt% TiCl 4 , has a high recovery value; in addition, niobium is a common associated element in titanium-rich materials. After carbon reduction and chlorination of titanium-rich materials, more than 90% of niobium is enriched in the crude titanium tetrachloride precipitation slurry. In order to recover TiCl in crude titanium tetrachloride precipitation mud 4 , production enterprises and scientific research institutions have conducted a lot of research and attempts, including: the sedimentation mud is returned to the boi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/02C01G33/00
Inventor 王学文向小艳王明玉
Owner CENT SOUTH UNIV