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Method and equipment for continuous preparation of high-purity titanium by oxide melting electrolysis-vacuum rectification

A technology of molten electrolysis and vacuum distillation, applied in the direction of electrolysis components, electrolysis process, electrodes, etc., can solve the problems of high energy consumption and low production efficiency of electrolysis, and achieve the effect of wide sources, low production cost and high-efficiency production

Active Publication Date: 2021-02-12
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the electrolysis energy consumption of this method is too high, and the two-step electrolysis is adopted, the production efficiency is low, and the product needs to be further processed

Method used

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  • Method and equipment for continuous preparation of high-purity titanium by oxide melting electrolysis-vacuum rectification

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: adopt tin as cathode, iron-chromium alloy as anode, titanium-containing oxide slag (25.35wt% CaO, 14.83wt% Al 2 o 3 , 7.84wt% MgO, 23.41wt% SiO 2 and 28.57wt% TiO 2 ) is the electrolyte. Raise the temperature to 1550°C, pre-melt for 3 hours, then lower the anode into the electrolyte, and simultaneously energize the anode and cathode to start constant current electrolysis with a current density of 3A cm -2 ; During the electrolysis process, argon is passed through the electrolysis furnace for protection.

[0025] Step 2: Monitor the titanium ion activity in the titanium-containing oxide slag and the tin-titanium alloy. When the titanium ion activity in the titanium-containing oxide slag is less than 8%, open the slag outlet to discharge the slag, and open the slag delivery port to send the slag at the same time. Ensure that the titanium ion activity in the titanium-containing oxide slag is between 6 and 80%; at the same time, when the titanium ion activity in...

Embodiment 2

[0028] Step 1: Using antimony as the cathode, graphite as the anode, titanium oxide slag (19.54wt% CaO, 21.46wt% Al 2 o 3 , 4.21wt% MgO, 11.09wt% SiO 2 ,16.32wt%TiO 2 and 27.38 wt% CaF 2 ) is the electrolyte. Raise the temperature to 1400°C, pre-melt for 2 hours, then lower the anode into the electrolyte, and simultaneously energize the anode and cathode to start constant current electrolysis with a current density of 6A cm -2 ; During the electrolysis process, argon is passed through the electrolysis furnace for protection.

[0029] Step 2: Monitor the titanium ion activity in the titanium-containing oxide slag and the antimony-titanium alloy cathode. When the titanium ion activity in the titanium-containing oxide slag is less than 8%, open the slag outlet to discharge the slag, and simultaneously open the slag delivery port to send the slag. Always ensure that the titanium ion activity in the titanium-containing oxide slag is between 6 and 80%; at the same time, when th...

Embodiment 3

[0032] Step 1: adopt lead-bismuth alloy as cathode, iron-chromium alloy as anode, titanium oxide slag (32.11wt% CaO, 22.34wt% Al 2 o3 , 13.67wt% MgO, 6.21wt% SiO 2 and 25.67wt% TiO 2 ) is the electrolyte. Raise the temperature to 1500°C, perform pre-melting for 1 hour, then lower the anode into the electrolyte, and simultaneously energize the anode and cathode to start electrolysis at a constant voltage of 5V; during the electrolysis process, helium gas is passed through the electrolysis furnace for protection.

[0033] Step 2: Monitor the titanium ion activity in the titanium-containing oxide slag and the lead-bismuth-titanium alloy cathode. When the titanium ion activity in the titanium-containing oxide slag is less than 8%, open the slag outlet for slag discharge, and open the slag delivery port to send slag , and always ensure that the titanium ion activity in the titanium-containing oxide slag is between 6 and 80%; at the same time, when the titanium ion activity in the...

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Abstract

The invention relates to a method and equipment for continuous preparation of high-purity titanium by oxide melting electrolysis-vacuum rectification, belonging to the fields of electrochemical metallurgy and vacuum metallurgy. The process steps are as follows: add metal or alloy cathode and titanium-containing oxide slag electrolyte in the electrolytic furnace, use inert electrode or graphite as the anode; perform electrolysis under high temperature conditions, and send the titanium-containing alloy obtained by electrolysis into the rectification furnace for rectification , Separation of titanium and metal or alloy cathode; making the metal or alloy cathode return to the electrolytic furnace through evaporation to realize circulation. The entire operation process realizes the continuous preparation of high-purity titanium by controlling the rectification furnace and electrolytic furnace to realize oxide melting electrolysis-vacuum rectification. The invention meets the requirements of green metallurgy, utilizes the principles of electrochemical metallurgy and vacuum metallurgy, continuously and comprehensively recovers metallurgical secondary resources, and has the advantages of low energy consumption, simple operation, short process and the like.

Description

technical field [0001] The invention relates to a method and equipment for continuous preparation of high-purity titanium by oxide melting electrolysis-vacuum rectification, belonging to the fields of electrochemical metallurgy and vacuum metallurgy. Background technique [0002] Due to its high specific strength, corrosion resistance and good biocompatibility, titanium is considered as a future metal and is widely used in aerospace, petrochemical, nuclear power, ships, submarines and biomedicine. It accounts for about 0.42% in the earth's crust, which is 16 times the total amount of copper, nickel, lead, and zinc. However, most titanium-containing minerals are composite ores, which are difficult to directly smelt. At present, the Kroll method is the main industrial production method of titanium. While producing titanium, this method has high requirements for intermediates such as titanium tetrachloride and magnesium, and has strict requirements for the airtightness and pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C3/28C25C7/02C22B9/02C22B34/12
CPCC22B9/02C22B34/1295C25C3/28C25C7/025
Inventor 焦树强蒲正浩王明涌焦汉东
Owner UNIV OF SCI & TECH BEIJING
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