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Two-step method for preparing high-purity titanium

A high-purity, one-step technology, applied in the field of high-purity titanium preparation from molten salt, can solve the problems of long process, low product quality, high energy consumption, etc., and achieve the effect of improving quality and low production cost

Active Publication Date: 2017-07-14
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to: overcome the disadvantages of long process, high energy consumption, product quality not up to the standard of high-purity titanium or the inability to realize industrialization in the method for producing metal titanium in the prior art, and provide a two-step method for preparing high-purity titanium The method has the advantages of simple process, low energy consumption and the method of industrialized extraction of high-purity titanium

Method used

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  • Two-step method for preparing high-purity titanium

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Effect test

Embodiment 1

[0025] Mixed oxide TiO 2 +MgO+Al 2 o 3 +CaO and CaF with a mass fraction of 10% 2 additives as electrolytes, where TiO 2 The mass percentage is 20%. Mix the electrolyte evenly and place it at the bottom of the reaction vessel, insert the graphite anode and the metal molybdenum cathode, cover the reaction device and perform sealing treatment. After evacuating, the inert protective atmosphere of argon is introduced, and argon protection is maintained at a certain flow rate. After the atmosphere in the reaction device is stabilized, the reaction device is heated to 1500 ° C at a rate of 300 ° C / hour and kept for 3 hours, so that The electrolyte is in a uniform melting state, ensuring uniform temperature distribution in the reaction device. The graphite anode was then slowly inserted into the molten electrolyte with a cathodic current density of 0.5 A / cm 2 Constant current electrolysis for 2 hours. After the electrolysis is completed, the cathode product is collected, was...

Embodiment 2

[0028] Mixed oxide TiO 2 +MgO+Al 2 o 3 +CaO and 10% LiF additive as the electrolyte, in which TiO 2 The mass percentage is 50%. Mix the electrolyte evenly and place it at the bottom of the reaction vessel, insert the SnO 2 An inert anode and a metal nickel cathode are covered with a reaction device cover and sealed. After evacuating, argon gas is introduced into the inert protective atmosphere, and argon protection is maintained at a certain flow rate. After the atmosphere in the reaction device is stabilized, the reaction device is heated to 1700°C at a rate of 300°C / hour and kept for 3 hours, so that The electrolyte is in a uniform melting state, ensuring uniform temperature distribution in the reaction device. The graphite anode was then slowly inserted into the molten electrolyte with a cathodic current density of 0.5 A / cm 2 Constant current electrolysis for 2 hours. After the electrolysis is completed, the cathode product is collected, washed repeatedly with hydroc...

Embodiment 3

[0031] Mixed oxide TiO 2 +MgO+Al 2 o 3 +CaO and 5% LiF+NaF (50:50% by mass) additives as electrolytes, in which TiO 2 The mass percentage is 30%. Mix the electrolyte evenly and place it at the bottom of the reaction vessel, insert the graphite anode and the metal titanium cathode, cover the reaction device and perform sealing treatment. After evacuating, the inert protective atmosphere argon is introduced, and argon protection is maintained at a certain flow rate. After the atmosphere in the reaction device is stable, the reaction device is heated to 1600 ° C at a rate of 300 ° C / hour and kept for 3 hours, so that The electrolyte is in a uniform melting state, ensuring uniform temperature distribution in the reaction device. Then the graphite anode was slowly inserted into the molten electrolyte, and a 5V direct current was applied for electrolysis for 2 hours. After the electrolysis is completed, the cathode product is collected, washed repeatedly with hydrochloric aci...

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Abstract

The invention provides a two-step method for preparing high-purity titanium, and relates to the field of electrochemical metallurgy. The two-step method includes the two steps of preparation of low-valence TiOx (x<1) and extraction of high-purity titanium. Firstly, a TiOx (x<1) raw material is prepared with graphite or an inert electrode as the anode and a metal material as a cathode in an electrolyte system with oxides (TiO2+MgO+Al2O3+CaO) and a small quantity of fluorides as additives; and then in a chloride electrolyte system, high-purity titanium is extracted through fused salt with TiOx as the anode and a metal material as a cathode, and in the process, free-state [O] generated in an electrolyte can further oxide residual low-valence TiOx into high-valence TiO2 which returns to the first step to serve as an oxide titanium ion source raw material. The novel two-step method for extracting high-purity titanium through fused salt has the characteristics that the technique is simple, energy consumption is low and the titanium recovery rate is high, and can achieve industrial extraction of high-purity titanium.

Description

technical field [0001] The invention relates to a method for preparing high-purity titanium from molten salt, especially using low-priced TiO x (x<1) is a raw material, belongs to the field of electrochemical metallurgy, and can specifically realize a method for preparing high-purity titanium from oxides containing low-valent titanium ions. Background technique [0002] Due to its stable chemical properties, good high temperature resistance, low temperature resistance, strong acid and alkali resistance, high strength and low density, titanium metal is known as "space metal" and "ocean metal". At present, titanium metal has become an excellent lightweight structural material, a new type of functional material and an important biomedical material. Pure titanium generally refers to titanium materials with a purity (mass fraction) greater than 99%, while the purity of high-purity titanium can reach 4N grade (99.99%) or even higher. As a member of titanium series products, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/12C25C3/28
CPCC22B34/1277C25C3/28
Inventor 焦树强王帅朱俊
Owner UNIV OF SCI & TECH BEIJING
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