Improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder

A technology of titanium tetrachloride and titanium trichloride, applied in the directions of titanium tetrachloride, titanium halide, etc., can solve the problems of reducing the recovery rate of titanium tetrachloride, large amount of vanadium-removing residue liquid, and high energy consumption of the residue liquid, Achieve the effect of reducing the amount of vanadium removal residue liquid, less aluminum powder consumption, and faster vanadium removal.

Inactive Publication Date: 2015-03-18
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Vanadium removal reaction (2) is a solid-liquid reaction, VOCl 3 (liquid phase) by 3TiCl 3 ·AlCl 3 TiCl in compound (solid phase) 3 Reduction to VOCl 2 (solid phase) and deposited on 3TiCl 3 ·AlCl 3 compound surface, while its internal TiCl 3 It cannot be utilized because it is wrapped by the reaction product, resulting in TiCl 3 The utilization rate of the vanadium is extremely low, that is, the consumption of aluminum powder in the process of removing vanadium is large, which is 5 to 10 times the theoretical amount of the reaction.
The large consumption of aluminum powder results in a large amount of vanadium removal residue solution, high energy consumption for processing a large amount of residue solution, and at the same time reduces the recovery rate of titanium tetrachloride

Method used

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  • Improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder
  • Improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder
  • Improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of TiCl 3 slurry test

[0030] Install a reflux condenser on a 500ml flask, add raw materials in the flask, including refined TiCl 4 , AlCl 3 and aluminum powder, heat the flask on an electric furnace to make the reactant mixture boil, the evaporating product is condensed in the condenser and refluxed into the flask, when the reactant boils for a period of time, purple-red TiCl appears 3 , indicating that the reaction has started, and then maintain the boiling state for a certain period of time to complete the reaction. After the reaction is completed, it is cooled to TiCl 3 Slurry, with refined TiCl 4 Cleaning is transferred to containers and metered.

[0031] Prepare two TiCl according to the raw material composition listed in Table 1 3 Slurry sample, in which 1#TiCl 3 Slurry without any treatment; 2#TiCl 3 The slurry was prepared by ball milling in a ball mill tank for 4 hours at a milling speed of 60 rpm. The test results are liste...

Embodiment 2

[0040] Embodiment 2: TiCl treated by ball milling 3 Vanadium removal test of slurry

[0041] Ball-milled TiCl 3 The operating process of the vanadium removal test of the slurry is the same as that of Comparative Example 1, except that the 2# TiCl prepared in Example 1 is processed through ball milling 3 Slurry replaces untreated 1# TiCl 3 slurry. Ball-milled TiCl 3 The vanadium removal test results of the slurry are listed in Table 3.

[0042] Table 3 TiCl treated by ball milling 3 Slurry vanadium removal test results

[0043]

Embodiment 3

[0049] Embodiment 3: the vanadium removal test of the still residue liquid of ball milling treatment

[0050] The operation process of removing vanadium is the same as that of Comparative Example 2, and the raw material crude TiCl 4 (VOCl 3 Content 0.21%) was added and ball milled in a ball mill tank for 4 hours at a ball milling speed of 60 rpm, and the activated still residue liquid was used for vanadium removal. The test results are listed in Table 5.

[0051] Table 5 Test results of vanadium removal in industrial production kettle residue liquid by ball milling

[0052]

[0053] In addition to ball milling, other mechanical pulverizing and grinding methods can also be used in the refinement and activation treatment of the present invention, such as rod mills and sand mills, or ultrasonic pulverization methods, all of which can achieve the same effect as ball milling.

[0054] It can be seen from comparative example 1 and embodiment 2 that the TiCl treated by ball mill...

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Abstract

The invention relates to an improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder. The improvement method comprises the following steps: by adopting AlCl3 as a catalyst, reacting TiCl4 with aluminum powder to prepare TiCl3 slurry, then performing refining and activation treatment on the produced TiCl3 slurry, and removing vanadium impurities from TiCl4 by using the treated TiCl3 slurry; or performing refining and activation treatment on a vanadium removal residue liquid which is produced by removing vanadium by virtue of aluminum powder, and then removing the vanadium impurities from TiCl4 again by using the treated residue liquid. The improvement method for removing vanadium by virtue of the aluminum powder, disclosed by the invention, has the advantages of high vanadium removal speed and small aluminum powder consumption, and the quantity of the vanadium removal residue liquid can be greatly reduced, so that the improvement method is an efficient method with low cost, high recovery rate and less three-waste quantity.

Description

technical field [0001] The invention relates to a method for removing vanadium impurities in titanium tetrachloride, in particular to an improved method for continuously removing vanadium impurities in titanium tetrachloride by using aluminum powder as a reducing agent. Background technique [0002] Titanium tetrachloride is the raw material for the production of sponge titanium by the Krall method and the production of titanium dioxide by the chloride method. There are many harmful impurities in the crude titanium tetrachloride produced by chlorination of titanium-containing raw materials. These impurities directly affect the quality of sponge titanium and titanium dioxide. Therefore, crude titanium tetrachloride must be purified before it can be used to produce sponge titanium and titanium dioxide. Titanium dioxide. Most of the impurities in the crude titanium tetrachloride can be separated and removed by sedimentation filtration, distillation and rectification, but the v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
CPCC01G23/024
Inventor 刘水根邓国珠薛红霞
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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