Method for preparing high-purity titanium through calcium in-situ distillation-deoxygenation

A high-purity, in-situ technology, applied in the field of metal smelting, can solve problems such as high energy consumption and pollution of titanium products, and achieve the effects of reducing energy consumption, high solubility, and reducing activity

Pending Publication Date: 2019-03-08
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first problem with this process is that during the packaging, storage and transportation of the high-purity calcium obtained by distillation, the high-purity calcium will introduce nitrogen and oxygen impurities due to the absorption of oxygen, nitrogen a

Method used

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  • Method for preparing high-purity titanium through calcium in-situ distillation-deoxygenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 1 metal titanium plate with a mass of 15g and an oxygen content of 850ppm, press (CaCl 2 ): m(Ti)=40:1 Weigh 600g of anhydrous calcium chloride (dehydrated at 600°C for 36 hours before use), weigh 60g of high-purity calcium chips (at 1300°C, calcium in anhydrous calcium chloride molten salt 0.5 times the saturation solubility), metal titanium and anhydrous calcium chloride are filled in the titanium crucible, high-purity calcium chips are filled in the gap between the titanium crucible and the superalloy crucible, and then the superalloy crucible is sealed with a high temperature sealing gasket In good condition, as attached figure 1 shown.

[0037] Put the sealed crucible into a high-temperature alloy vacuum tank heated by a resistance furnace, cover the furnace cover, evacuate to 0.2 Pa, and then wash with argon. Under the protection of argon, heat up to 1300°C at 5°C / min, and keep at 1300°C for 12 hours. After the heat preservation is over, the furnace is cool...

Embodiment 2

[0039] Take 1 metal titanium plate with a mass of 22g and an oxygen content of 840ppm, press (CaCl 2 ): m(Ti)=20:1 Weigh 440g of anhydrous calcium chloride (dehydrated at 500°C for 24 hours before use), and weigh 176g of distilled calcium chips (at 1300°C, calcium saturated in anhydrous calcium chloride molten salt 2 times the solubility), metal titanium and anhydrous calcium chloride are filled in the titanium crucible, and the distilled calcium chips are filled in the gap between the titanium crucible and the high-temperature alloy crucible, and then the high-temperature alloy crucible is sealed with a high-temperature sealing gasket. Specific as attached figure 1 shown.

[0040] Put the sealed crucible into a high-temperature alloy vacuum tank heated by a resistance furnace, cover the furnace cover, evacuate to 0.2 Pa, and then wash with argon. Under the protection of argon, heat up to 1300°C at 5°C / min, and keep at 1300°C for 12 hours. After the heat preservation is over...

Embodiment 3

[0042] Get 1 metal titanium wire, quality 15g, oxygen content 690ppm, according to (CaCl 2 ): m(Ti)=30:1 Weigh 450g of anhydrous calcium chloride (dehydrated at 400°C for 30h before use), weigh 146g of industrial calcium chips (at 1000°C, calcium saturated in anhydrous calcium chloride molten salt 5 times of the solubility), metal titanium and anhydrous calcium chloride are filled in the titanium crucible, industrial calcium chips are filled in the gap between the titanium crucible and the stainless steel crucible, and then the stainless steel crucible is sealed with a high-temperature sealing gasket, specifically as follows attached figure 1 shown.

[0043] Put the sealed crucible into a vacuum tank heated by a resistance furnace, cover the furnace cover, vacuumize to 0.4 Pa, and then wash with argon. Under the protection of argon, heat up to 1000°C at 5°C / min, and keep it at 1000°C for 48 hours. After the heat preservation is over, the furnace is cooled to room temperature...

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Abstract

The invention discloses a method for preparing high-purity titanium through calcium in-situ distillation-deoxygenation, and belongs to the technical field of metal smelting. The method comprises the steps that a raw material system A and a calcium reducing agent are placed in a closed reaction vessel in a partitioned manner, heating is carried out in an inert atmosphere, calcium in the calcium reducing agent is dissolved to enter molten salt in the raw material system A in the form of high-purity calcium gas, deoxygenation of a titanium raw material is achieved, and the high-purity titanium with the oxygen content being smaller than or equal to 0.10% by weight is prepared; the raw material system A is a mixture of the titanium raw material and anhydrous calcium chloride, the raw material system A contains or does not contain one or two of alkali metal halide or alkaline earth metal halide, and the titanium raw material is titanium metal or titanium oxide; the calcium reducing agent ismetal calcium or a calcium alloy; and partitioned regions for partitioned containing are separated from each other and are in gas phase communication. The method is simple and easy to perform, has thegood oxygen and nitrogen removing effect, can meet the using requirements in the fields of aerospace, national defense military and the like.

Description

technical field [0001] The invention belongs to the technical field of metal smelting, in particular to a method for preparing high-purity titanium by calcium in-situ distillation-deoxidation. Background technique [0002] Titanium has the advantages of low density, high strength, non-magnetism, corrosion resistance, and easy processing and forming. It has become the "third metal" after iron and aluminum. Therefore, some people predict that the 21st century will be the century of titanium. Titanium alloys are currently widely used in aerospace, national defense and military industry, chemical metallurgy, seawater desalination, biomedicine and other fields. The United States and Russia are countries with a long history of titanium research and the strongest strength in the world. The application of titanium materials has always been dominated by the aerospace market, and the civilian industry is relatively small. China is different, and the non-aerospace market accounts for a...

Claims

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Application Information

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IPC IPC(8): C22B5/04C22B5/12C22B34/12
CPCC22B5/04C22B5/12C22B34/1268
Inventor 王力军马朝辉张建东黄永章张顺利闫国庆段锦
Owner 有研资源环境技术研究院(北京)有限公司
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