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
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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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