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Method for preparing titanium sponge through magnesium and chlorine recycling

A technology of sponge titanium and titanium tetrachloride, applied in the direction of improving process efficiency, can solve the problem of high investment in magnesium and chlorine cycle equipment, and achieve the effects of reducing economic benefits, reducing production costs, and reducing equipment investment.

Active Publication Date: 2011-09-14
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned patented technologies can improve the technical level of titanium sponge production to a certain extent, they cannot fundamentally solve the problems of high investment in magnesium and chlorine cycle equipment in the production process of titanium sponge.

Method used

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  • Method for preparing titanium sponge through magnesium and chlorine recycling
  • Method for preparing titanium sponge through magnesium and chlorine recycling

Examples

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Effect test

Embodiment 1

[0036]Example 1: Firstly, the natural rutile was crushed and finely ground to -0.25mm, and then crude titanium tetrachloride was obtained under the conditions of chlorination temperature of 800°C, chlorination time of 60min, and operating fluidization number of 10. The crude titanium tetrachloride was obtained by After iron removal in a distillation tower with a bottom temperature of 140°C and a top temperature of 137°C, silicon is removed through a rectification tower with a bottom temperature of 140°C and a top temperature of 57°C, and then vanadium is removed with copper wire at a temperature of 136°C , to obtain a titanium tetrachloride product with a purity greater than 99wt%, the refined titanium tetrachloride and metal magnesium are in a ratio of 1.3:1 according to the mass ratio of magnesium and titanium, the reaction temperature is 700 ° C, and the reaction time is 8 hours, and sponge titanium and magnesium chloride and The mixture of silicon tetrachloride, distilling ...

Embodiment 2

[0037] Example 2: Firstly, the natural rutile is crushed and finely ground to -0.25mm, and then crude titanium tetrachloride is obtained under the conditions of chlorination temperature of 1050°C, chlorination time of 10min, and operating fluidization number of 5. The crude titanium tetrachloride is obtained by using After removing iron in the distillation tower with a bottom temperature of 145°C and a top temperature of 137°C, silicon is removed through a rectification tower with a bottom temperature of 140°C and a top temperature of 70°C, and then copper wire is used to remove vanadium at a temperature of 140°C , to obtain a titanium tetrachloride product with a purity greater than 99wt%, the refined titanium tetrachloride and metal magnesium are in a ratio of 1.8:1 according to the mass ratio of magnesium and titanium, the reaction temperature is 1000°C, and the reaction time is 5h, and sponge titanium and magnesium chloride and The mixture of silicon tetrachloride, the mixt...

Embodiment 3

[0038] Example 3: Firstly, the high titanium slag was crushed and finely ground to -0.25mm, and then crude titanium tetrachloride was obtained under the conditions of chlorination temperature of 900°C, chlorination time of 40min, and operating fluidization number of 7, crude titanium tetrachloride After iron removal by a distillation tower with a bottom temperature of 142°C and a top temperature of 137°C, silicon is removed by a rectification tower with a bottom temperature of 140°C and a top temperature of 60°C, and then copper wire is used to remove silicon at a temperature of 138°C. Vanadium, to obtain titanium tetrachloride products with a purity greater than 99wt%, the refined titanium tetrachloride and metal magnesium are in a ratio of 1.5:1 according to the mass ratio of magnesium and titanium, the reaction temperature is 900 ° C, and the reaction time is 6 hours to obtain sponge titanium and magnesium chloride The mixture of sponge titanium, magnesium chloride and silic...

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Abstract

The invention relates to the technical field of preparation of nonferrous metal, in particular to a method for preparing titanium sponge through magnesium and chlorine recycling. The method comprises the following steps of: crushing natural rutile or titanium-rich slag, finely grinding to -0.25mm and chlorinating to obtain rough titanium tetrachloride; removing iron from the rough titanium tetrachloride by using a distillation tower with bottom temperature of between 140 DEG C and 145 DEG C and top temperature of 137 DEG C; removing silicon through a rectification tower with bottom temperature of 140 DEG C and top temperature of between 57 DEG C and 70 DEG C; removing vanadium by using copper wires to obtain a titanium tetrachloride product with purity of more than 99 percent; proportioning refined titanium tetrachloride and metal magnesium according to a mass ratio of magnesium to titanium as (1.3:1)-(1.8:1) and reacting at the temperature of between 700 DEG C and 1,000 DEG C to obtain mixture of the titanium sponge, the magnesium chloride and the silicon tetrachloride; and distilling the mixture of the titanium sponge, the magnesium chloride and the silicon tetrachloride for 30-35 hours under the conditions of temperature of between 880 DEG C and 1,000 DEG C and final vacuum degree of less than 0.1Pa to separate the titanium sponge and the magnesium chloride.

Description

technical field [0001] The invention relates to the technical field of nonferrous metal preparation, in particular to a method for preparing sponge titanium by recycling magnesium chloride. Background technique [0002] Titanium and titanium alloys have the advantages of low density, high specific strength, excellent corrosion resistance, and non-toxicity. It has been widely used in aerospace, chemical industry, metallurgy, light industry, shipbuilding, automobile, medicine, construction and other industries. [0003] At present, the industrial method of metal titanium production is the Kroll method, and the product of this method is titanium sponge. In the process of using the Kroll method to produce sponge titanium, first use chlorination (shaft furnace chlorination, molten salt chlorination, boiling chlorination, etc.) The titanium-containing phase transforms into TiCl 4 , the crude TiCl produced by the chlorination process 4 TiCl was purified by magnestic reduction ...

Claims

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Application Information

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IPC IPC(8): C22B34/12C22B5/04
CPCY02P10/20
Inventor 张廷安豆志河刘燕吕国志牛丽萍赵秋月赫冀成
Owner NORTHEASTERN UNIV
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