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A kind of ilmenite composite ore carbon vulcanization-electrolytic method for preparing titanium metal

A technology of metal titanium and titanium sulfide, applied in the direction of electrolytic components, electrolysis process, metal material coating process, etc., can solve the problems of excessive carbon content of carbon products, excessive carbon, high cost, etc., achieve less intermediate products, efficient recycling, The effect of high electrolysis efficiency

Active Publication Date: 2020-02-28
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following problems in this method: the cost of raw material is higher, all adopts titanium tetrachloride and metal titanium, and the reduction reaction rate of titanium tetrachloride is lower
This method has the following problems: the amount of carbon added is excessive, and there will still be carbon residues and excessive carbon content in the product in the electrolysis process
It can be seen from the above that titanium sulfide can be used in the electrolyte molten salt to obtain metal titanium, but it is used in the cathode area instead of being soluble as the anode.

Method used

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  • A kind of ilmenite composite ore carbon vulcanization-electrolytic method for preparing titanium metal
  • A kind of ilmenite composite ore carbon vulcanization-electrolytic method for preparing titanium metal
  • A kind of ilmenite composite ore carbon vulcanization-electrolytic method for preparing titanium metal

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preparation example Construction

[0044] (1) Low-cost preparation and synthesis of titanium sulfide (TiS) with metal conductivity 2 , TiS, Ti 2 S, Ti 3 S, Ti 6 S and Ti 4 S 5 Wait);

[0045] (2) The titanium sulfide can be prepared by processing titanium-containing concentrates, which effectively solves the problem of stacking and discarding titanium-containing ores such as vanadium-titanium magnetite and the like;

[0046] (3) Titanium sulfide is used as a soluble anode. During the electrolysis process, titanium is dissolved in the electrolyte in the form of ions, and sulfur is discharged from the anode in the form of sulfur gas for recycling, effectively realizing the efficient and comprehensive utilization of resources and energy;

[0047] (4) Due to the weak affinity between titanium and sulfur, metal titanium can be obtained at a higher rate without re-contamination;

[0048] (5) Direct electrolysis in the electrolyte can deposit metal titanium with low oxygen content at the cathode.

[0049] In S2...

specific Embodiment 1

[0053] Titanium dioxide (TiO 2 , 99.5wt%), graphite powder (99.95), sulfur powder (99%) is prepared according to the molar ratio of 1:2:2.1, a total of 100g.

[0054] Mix and grind in a spherical ball mill for 12 hours, weigh 5g and press it into a small piece with a diameter of 5mm*5mm under a pressure of 10Mpa, and place it in a closed glass tube at one end, and seal it with high-temperature resistant organic glue to ensure that the glass tube No air leakage at high temperature.

[0055] Then place the glass tube in a muffle furnace, burn it at 1000 °C for 10 h, then lower the temperature to room temperature, cut the glass tube and take out the synthesized TiS 2 Material. Synthesized TiS 2 The XRD diffraction pattern of the material is attached figure 2 shown.

[0056] Then use vacuum high temperature (1100°C) to treat TiS 2 The material is sintered to obtain a cylindrical anode with a diameter of 10mm*15mm.

[0057] A corundum crucible containing 150 g of NaCl-KCl e...

specific Embodiment 2

[0060] For 500g of titanium concentrate FeTiO 3 Sulfurization treatment is carried out at 1200°C, and the processed products are FeS and TiO 2 Mix powder.

[0061] The mixed powder was soaked in 1mol / L dilute hydrochloric acid, and vacuum filtered, then dried in an oven at 80°C to obtain titanium dioxide (TiO 2 ).

[0062] Titanium dioxide (TiO 2 , 99.5wt%), graphite powder (99.95), sulfur powder (99%) is prepared according to the molar ratio of 1:2:2.2, a total of 10g.

[0063] Mix and grind in a spherical ball mill for 12 hours, weigh 2 g and press it into a small piece with a diameter of 5mm*5mm under a pressure of 10Mpa, and place it in a closed glass tube at one end, and seal it with high-temperature resistant organic glue to ensure that the glass tube In a sealed state, there is no air leakage under high temperature.

[0064] Then place the glass tube in a muffle furnace, burn it at 1000°C for 10 h and then lower the temperature to room temperature, cut the glass tu...

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Abstract

The invention provides a method for preparing titanium metal by ilmenite composite ore carbon sulfide-electrolysis, which relates to the technical field of non-ferrous metal extraction. It adopts titanium sulfide anode for electrolysis, and has the advantages of high electrolysis efficiency, less intermediate products, and high-purity titanium directly. Advantages, it can also be produced continuously without producing anode slime, and realizes efficient recycling of energy minerals; the method steps include S1, mixing titanium-containing materials, carbon-containing reducing agents, and sulfur-containing reducing agents in a molar ratio of 1:2.0:2.0 ~1:2.5:3.0 ratio is uniformly mixed to make a mixture, and the mixture is completely vulcanized to prepare a titanium sulfide product; S2, prepare the titanium sulfide product into a solid solution; S3, in a molten salt electrolyte system Metal titanium is extracted by electrolysis, the anode is the solid solution during electrolysis, the anode recovers sulfur gas, and the cathode obtains metal titanium. The technical scheme provided by the invention is suitable for the processes of sulfidation of titanium-containing ores and electrochemical extraction of metallic titanium.

Description

【Technical field】 [0001] The invention relates to the technical field of non-ferrous metal extraction, in particular to a method for preparing titanium metal by ilmenite composite ore-carbon vulcanization-electrolysis. 【Background technique】 [0002] Due to its excellent physical and chemical properties, titanium metal is widely used in aviation, aerospace, petroleum, chemical industry, automobile, medical equipment, civil construction and other fields, and is known as "future metal" and "strategic metal". [0003] Titanium raw materials are mainly ilmenite and rutile concentrate, followed by white titanium ore, anatase and red titanium ore. According to the 2018 statistics released by international authoritative organizations: the global ilmenite reserves are 970 million tons, and the rutile reserves are 62 million tons. my country's titanium resources (TiO 2 ) is very rich, mainly vanadium-titanium magnetite and ilmenite, of which vanadium-titanium magnetite accounts for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C3/28C25C7/02
CPCC25C3/28C25C7/025B22F2999/00B22F9/20Y02P10/20C22C1/05C23C8/08
Inventor 焦树强田栋华焦汉东
Owner UNIV OF SCI & TECH BEIJING
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