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Process of preparing titanium sponge by fusion electrolysis of titanium dioxide

A technology of titanium dioxide and molten salt electrolysis, applied in the field of non-ferrous metal materials, can solve the problems of low current efficiency of sponge titanium

Inactive Publication Date: 2005-09-07
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is aimed at the current molten salt electrolysis of TiO 2 Due to the disadvantage of low current efficiency in preparing titanium sponge, a method for preparing titanium sponge by molten salt electrolysis of titanium dioxide is proposed, which has high current efficiency

Method used

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Examples

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Effect test

Embodiment 1

[0008] Embodiment 1, the cathode is made of a titanium dioxide sintered plate, which is made of titanium dioxide plus a weight percentage of 2% PVA binder and pressed into a plate shape under a carbon reducing atmosphere and baked at 1250 ° C for 2 hours; the anode is made of an inert material; A mixed electrolyte of calcium chloride and lithium chloride is used in the electrolysis process, wherein the lithium chloride content is 5% by weight, and the electrolysis temperature is 850°C. In electrolysis, the cell voltage is controlled at 2.9V, oxygen ions escape from the cathode, and the oxygen ions move towards the anode under the action of an electric field. Oxygen is generated by discharging on the anode, electrolyzed for 4 hours, and the oxygen content in the cathode is 600ppm, and it becomes titanium sponge. The vertical arrangement of the cathode and the anode increases the electrolysis area and improves the productivity of a single cell, and the current efficiency is 70%....

Embodiment 2

[0009] Example 2, the cathode of the electrolytic cell is made of titanium mesh, containing titanium dioxide particles, the mesh is 150 mesh, containing titanium dioxide particles, with a diameter of 2 mm, and the titanium dioxide particles are made of titanium dioxide powder plus water pellets, and are roasted at 1200 ° C for 1 hour under a carbon reducing atmosphere The anode is made of graphite; a mixed electrolyte of calcium chloride and lithium chloride is used in the electrolysis process, wherein the weight percentage of lithium chloride is 15%, and the electrolysis temperature is 870°C. In the electrolysis, the cell voltage is controlled at 3.0V, and the working process is the same as in Example 1, except that the gas released on the anode is carbon dioxide, and the oxygen content in the cathode is 500ppm, which becomes titanium sponge. Open the titanium mesh, take out the titanium sponge, and the current efficiency is 80%.

Embodiment 3

[0010] Example 3, the cathode of the electrolytic cell is made of stainless steel mesh, with titanium dioxide particles inside, the mesh is 200 mesh, and titanium dioxide particles are inside, with a diameter of 5mm. The titanium dioxide particles are made of titanium dioxide powder plus water pellets, and are baked at 1300 ° C under a carbon reducing atmosphere 2h; the anode is made of graphite; a mixed electrolyte of calcium chloride and lithium chloride is used in the electrolysis process, wherein the percentage content of lithium chloride is 20%, and the electrolysis temperature is 900°C. In the electrolysis, the cell voltage is controlled at 2.8V, and the working process is the same as in the first embodiment, except that the gas released on the anode is carbon dioxide, and the oxygen content in the cathode is 500ppm, which becomes titanium sponge. Open the stainless steel mesh and take out the titanium sponge, the current efficiency is 80%.

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Abstract

The invention relates to a method for preparing the titanium sponge through electrolyzing the titania by fused salt. The titania applied in the cathode is formed by roasting 1-3h in the carbon reducing atmosphere and 1200-1300 Deg.c. The cathode has two forms: one is plate-like titania, which is formed through roasting the shaped titania combined with PVA adhensive in high temperature and carbon reducing atmosphere; the second is titania particles, which is formed through roasting the rectangle mesh cathode made up of non-corrosive steel or metallic titanium netting in high temperature and carbon reducing atmosphere. The electrolyte is the mixing molten salt system of calcii chloridum and lithium chloride, and the anode uses carbite or inert materials. The cathode and anode are arranged vertically, and the electrode surfaces are parallel, and the electrolyser has at least one group of anode-cathode-anode electrode, and it can set many electrodes in one electrolyser. The voltage of the controlling electrolyzer is 2.8-3.2V, the electrolyzing temperature is 850-900 Deg.c. Cleaning the cathode with the dilute hydrochloric acid and drying it, and getting the titanium sponge, which contains oxygen below 600ppm and the current efficiency is between 70-80%.

Description

technical field [0001] The invention belongs to the field of non-ferrous metal materials, in particular to a method for preparing sponge titanium by molten salt electrolysis of titanium dioxide. Background technique [0002] The method commonly used in the production of sponge titanium industry in the world is the Kroll process, which is the reduction of TiCl by magnesium 4 Preparation of titanium sponge. This process has not changed much since its inception. The process consists of three parts: one is to prepare crude TiCl from titanium-containing minerals 4 ; The second is crude TiCl 4 Refining; the third is the reduction of TiCl by magnesium 4 Production of titanium sponge and vacuum distillation. The Kroll process is discontinuous, and the reaction must be loaded, heated at high temperature, and unloaded during the production process, which not only requires high energy consumption but also has a long cycle, high production costs, and serious environmental pollution...

Claims

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Application Information

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IPC IPC(8): C25C3/28
Inventor 卢惠民
Owner UNIV OF SCI & TECH BEIJING
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