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Method for directly preparing titanium and titanium alloy by titanium-containing waste residue

A technology of titanium waste slag and titanium alloy, which is applied in the field of electrochemical metallurgy, can solve the problems of waste slag discharge, waste slag ratio limitation, poor activity and viscosity, etc., and achieve the effect of improving current efficiency, avoiding re-oxidation, and increasing reduction speed

Inactive Publication Date: 2009-06-17
SHANGHAI UNIV
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Problems solved by technology

[0003] At present, some small-scale manufacturers directly discard the smoke dust, ferro-titanium slag, and superfine high-titanium slag. After the chlorinated slag is washed with lime water to hydrolyze the chloride, the residue is directly discharged. The treatment of chemical slag is mainly to select the titanium dioxide (artificial rutile) in it by washing with shaking table, and then mix the rutile into the chlorination charge to produce crude titanium tetrachloride. This method is labor intensive and the carbon particles in the slag cannot be obtained Until it is utilized, there is still a large amount of waste slag discharged after washing, and the activity of the obtained artificial rutile is low, which is also unfavorable to the stability of the chlorination production furnace.
The recycling and utilization of these waste slags have been reported at home and abroad, but they are limited to returning the mud generated in the chlorination and refining production to the chlorination furnace for recycling, while the dust from the electric furnace, ferro-titanium slag, and superfine high-titanium slag The treatment of waste residues such as chlorination slag and dust collection residue has its limitations based on the immaturity of the process itself, or the limitation of product use, and economic feasibility.
[0004] If the waste slag is directly returned to the titanium slag electric furnace for recycling, due to the poor activity and high viscosity of the waste slag, the addition of waste slag will reduce the air permeability in the smelting furnace, resulting in poor reaction in the furnace, prolonging the smelting time and increasing energy consumption. High, therefore, the proportion of waste slag returning to the electric furnace for smelting is limited, and the recovery rate is low

Method used

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  • Method for directly preparing titanium and titanium alloy by titanium-containing waste residue
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  • Method for directly preparing titanium and titanium alloy by titanium-containing waste residue

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: The iron-titanium slag in the waste slag was ball-milled in a high-energy ball mill for 2 hours, using liquid paraffin as a binder, and using a 24T powder press to press 2.5 g of slag powder into a disc with a diameter of 10 mm under a pressure of 6 MPa. After natural drying at room temperature, it was sintered in an oxidizing atmosphere at 1100°C for 2 hours. A molybdenum wire with a diameter of 0.2 mm is used to wind the disc on a molybdenum rod with a diameter of 1.5 mm to make a cathode; the anode is a copper liquid saturated with carbon powder in a yttria-stabilized zirconia tube, and the CaCl 2 It is a molten salt electrolyte, and the graphite crucible is a reaction vessel. When the temperature of the furnace reaches 1100°C, insert the cathode into the molten salt in the crucible, and apply a voltage of 3.0-3.5V to the two poles for electrolysis. The electrolysis time is 6 hours. The electrolysis cathode product is rinsed and dried for detection. figu...

Embodiment 2

[0033] Example 2: Mill the high-titanium slag in the waste slag for 2 hours in a high-energy ball mill, use liquid paraffin as a binder, and use a 24T powder press to press 2.5 g of slag powder into a circle with a diameter of 10 mm under a pressure of 3 to 4 MPa. After natural drying at room temperature, the sheets were sintered in an oxidizing atmosphere at 1100°C for 2h. A molybdenum wire with a diameter of 0.2 mm is used to wind the disc on a molybdenum rod with a diameter of 1.5 mm to make a cathode; the anode is a copper liquid saturated with carbon powder in a yttria-stabilized zirconia tube, and the CaCl 2 It is a molten salt electrolyte, and the graphite crucible is a reaction vessel. When the temperature of the furnace reaches 1100°C, insert the cathode into the molten salt in the crucible, and apply a voltage of 3.0-3.5V to the two poles for electrolysis. The electrolysis time is 6 hours. The electrolysis cathode product is rinsed and dried for detection. Figure 4...

Embodiment 3

[0034] Example 3: Mill the high-titanium slag in the waste slag for 2 hours in a high-energy ball mill, use liquid paraffin as a binder, and use a 24T powder press to press 2.5 g of slag powder into a circle with a diameter of 10 mm under a pressure of 3 to 4 MPa. After natural drying at room temperature, the sheets were sintered in an oxidizing atmosphere at 1100°C for 2h. A molybdenum wire with a diameter of 0.2 mm is used to wind the disc on a molybdenum rod with a diameter of 1.5 mm to make a cathode; the anode is a copper liquid saturated with carbon powder in a yttria-stabilized zirconia tube, and the CaCl 2 It is a molten salt electrolyte, and the graphite crucible is a reaction vessel. When the furnace temperature reaches 1100°C, the cathode is inserted into the molten salt in the crucible, and a voltage of 3.0-3.5V is applied to the two poles for electrolysis. The electrolysis time is 4 hours. The electrolysis cathode product is washed and dried before detection. Im...

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Abstract

The invention relates to a method for directly preparing titanium and titanium alloy from titaniferous waste residues, and belongs to the technical field of electrochemical metallurgy. The method is characterized in that the titaniferous waste residues are made into an electrolysis electrode, and the electrolysis is performed in a crucible of an electrolytic cell by a solid oxygen permeable membrane in a specific molten salt electrolyte. The method comprises the following process steps: the titaniferous residues is processed by ball milling, then pressed and formed in a mould at 3-6MP, dried in the air, and then sinteredat the temperature of 1000-1100 DEG C for 2h to be made into an electrolysis cathode; molten salt is separated from an anode by an oxygen permeable membrane tube which only conducts oxyanion, the anode is liquid copper or copper alloy with saturated carbon powder, calcium chloride is taken as the molten salt electrolyte, the cathode and the anode are vertically arranged, the electrolytic temperature is 1000-1100 DEG C, the electrolytic voltage is 3.0-3.5V, the electrolysis time is 2-6h, and the cathodic products obtained by the electrolysis are metallic titanium and the titanium alloy. The method has the advantages of simple process, high electrolysis speed and high current efficiency.

Description

technical field [0001] The invention relates to a method for directly preparing titanium and titanium alloys from waste residue containing titanium, belonging to the technical field of electrochemical metallurgy. technical background [0002] In the production process from ilmenite to titanium tetrachloride, a large amount of waste residue will be generated. Including electric furnace fume, ferro-titanium slag, fine high-titanium slag, chlorinated furnace slag, dust collection residue, etc. According to statistics, every ton of titanium tetrachloride produces about 200 kg of waste slag, including 34 kg of soot, 18 kg of ferrotitanium slag, 46 kg of fine high-titanium slag, 40 kg of furnace slag, and 60 kg of dust collection slag. Thousands of tons of various waste residues are produced every year in my country's titanium industry. If these waste residues are not recycled, it will bring great problems to environmental protection and serious waste of resources. How to deal w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25C3/28C25C3/36
Inventor 陈朝轶鲁雄刚邹星礼华纬司新国刘宜强
Owner SHANGHAI UNIV
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