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Method for producing sodium tetrachloroaluminate by using TiCl4-containing material

A technology of sodium tetrachloroaluminate and materials, applied in aluminum chloride, aluminum halide and other directions, can solve problems such as inability to effectively separate and recycle, and achieve the effects of effective separation, environmental protection and production cost reduction

Inactive Publication Date: 2013-12-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In short, containing TiCl 4 AlCl in material 3 At present, it is not possible to effectively separate and recycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] containing TiCl 4 Add 500ml of 57.1%, Al6.3%, Fe1.2% titanium tetrachloride precipitation mud to a 1000ml three-necked flask, then press NaAlCl 4 Form 1.5 times the stoichiometric number by adding NaCl, and press FeCl 3 reduced to FeCl 2 Add iron powder three times the stoichiometric number, stir and evaporate at 160°C for 4 hours to obtain TiCl 4 Vapors and residues; TiCl will be obtained 4 -5°C liquid TiCl for steam 4 Spray recovery, recovered TiCl 4 The liquid contains 0.01% Al; and the evaporation residue is transferred to a vacuum furnace for vacuum distillation at a temperature of 250°C and a vacuum of 13 Pa for 3 hours; the NaAlCl produced by distillation 4 The purity of 99.7% NaAlCl is obtained after the steam is cooled at room temperature 4 Products; process aluminum recovery rate of 88.6%.

Embodiment 2

[0023] containing TiCl 4 Add 500ml of 61.6%, Al11.5%, Fe0.1% crude titanium aluminum tetrachloride powder to remove vanadium slag into a 1000ml three-necked flask, then press NaAlCl 4 Add NaCl to form twice the stoichiometric number, and evaporate at 200°C for 2.5 hours to obtain TiCl 4 Vapors and residues; TiCl will be obtained 4 -10°C liquid TiCl for steam 4 Spray recovery, recovered TiCl 4 The liquid contains 0.05% Al; and the evaporation residue is transferred to a vacuum furnace for vacuum distillation at a temperature of 300°C and a vacuum of 130Pa for 2.5 hours; the NaAlCl produced by distillation 4 The purity of 99.9% NaAlCl is obtained after the vapor is cooled at 150°C 4 Product, the evaporation rate of aluminum in the distillation process is 78.7%. The residue obtained by vacuum distillation contains a large amount of unreacted aluminum powder, which can be returned to the aluminum powder vanadium removal process for continued use.

Embodiment 3

[0025] containing TiCl 4 75.3%, Al8.7%, Fe0.5% crude titanium tetrachloride refining process produced the distillation residue 500ml into a 1000ml three-necked flask, and then press NaAlCl 4 Add NaCl to form 2.5 times the stoichiometric number, and press FeCl 3 reduced to FeCl 2 Add stannous chloride to 1.5 times the stoichiometric number, stir and evaporate at 250°C for 1 hour to obtain TiCl 4 Vapors and residues; TiCl will be obtained 4 -13°C liquid TiCl for steam 4 Spray recovery, recovered TiCl 4 The liquid contains 0.1% Al; and the evaporation residue is transferred to a vacuum furnace for vacuum distillation at a temperature of 400°C and a vacuum of 600Pa for 5 hours; the NaAlCl produced by distillation 4 After the steam is cooled at room temperature, the purity is 98.9% NaAlCl 4 Products, process aluminum recovery rate of 98.7%.

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Abstract

The invention discloses a method for producing sodium tetrachloroaluminate by using a TiCl4-containing material. The method is characterized by comprising the following steps: adding sodium chloride and a reducing agent into the TiCl4-containing material and evaporating TiCl4 by isolating air at 130 to 300 DEG C; and performing vacuum distillation on residues, obtained after the TiCl4 is evaporated, at 200 to 600 DEG C and recovering aluminum in the form of sodium tetrachloroaluminate. The method has the advantages that the process is simple; the production cost is low, the obtained sodium tetrachloroaluminate has high purity; the TiCl4 obtained by recovery has few impurities; and environmental friendliness is realized.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, in particular to a 4 Materials The method for producing sodium tetrachloroaluminate. Background technique [0002] Aluminum is an associated element in titanium concentrate. During the chlorination process of the titanium-rich material obtained from titanium concentrate, aluminum and titanium are chlorinated together. After the chlorination furnace gas is condensed, AlCl-containing 3 Crude TiCl 4 Liquid and precipitate containing solid aluminum chloride, the precipitate accounted for TiCl 4 3-5wt% of the total liquid, the sediment will form the so-called titanium tetrachloride precipitation mud in the crude titanium tetrachloride thickener, and the titanium tetrachloride precipitation mud is mainly composed of high-boiling chlorides and oxychlorides. Which contains 10-30wt% AlCl 3 , 0.2-5wt% FeCl 3 and 55-65wt% TiCl 4 , has a high recycling value. However, due to the special properties o...

Claims

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Application Information

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IPC IPC(8): C01F7/56
Inventor 王学文王明玉向小艳
Owner CENT SOUTH UNIV
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