Preparing method for titanium of Ti—C—S anode by carbonized/sulfurized ilmenite

Patent metadata

Field	Value
Publication number	US-11473207-B2
Application number	US-201916619892-A
Country	US
Kind code	B2
Filing date	Feb 28, 2019
Priority date	Nov 16, 2018
Publication date	Oct 18, 2022
Grant date	Oct 18, 2022

Abstract

Provided is a method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite, and relates to the technical field of mineral processing and electrochemical extraction of metallic titanium in molten salts in non-ferrous metallurgy. The method uses titanium-containing ore, carbon (C) and sulfur (S) as raw materials and prepares a Ti—C—S/titanium sulfide anode material with high electric conductivity through a sintering reaction, and then uses the Ti—C—S/titanium sulfide anode to prepare metallic titanium in a molten salt electrolyte system successfully. With the Ti—C—S composite soluble anode in the present invention, metallic titanium is deposited at the cathode and CS 2 /S 2 gas is generated at the anode in the molten salt electrolysis process; in addition, the gas can be used as a raw material to effectively treat the ore to prepare titanium sulfide.

First claim

The invention claimed is:

1. A method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite, comprising the following steps:
S1: sulfurizing a mixture comprising a titanium-containing material, a carbon-containing reducer and a sulfur reducer to prepare titanium sulfide;
S2: using the titanium sulfide and titanium carbide as raw materials to prepare a Ti—C—S composite;
S3: using the titanium sulfide or the Ti—C—S composite as an anode, and using electrochemical electrolysis to extract metallic titanium at the cathode; and
S4: collecting CS 2 and S 2 gasses generated by the anode during the electrolysis and using them for sulfurizing the titanium-containing material.

2. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the mixture is a mixture obtained by homogenously mixing the titanium-containing material, the carbon-containing reducer, and the sulfur reducer at a molar ratio of 1:2.0:2.0-1:2.5:3.0.

3. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the conditions of the sulfurization reaction in the step S1 include: burning reaction shielded by an inert atmosphere, temperature range in the reaction is 700° C. -1,600° C., and reaction time range is 30 min-900 min.

4. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein, in the step S2, the titanium sulfide and the titanium carbide are vacuum-sintered to prepare the Ti—C—S composite.

5. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein, during the electrolysis in the step S3, an electrolysis temperature is 70° C. -1,600° C., a spacing between the cathode and the anode is 1 cm-50 cm, a voltage range of the electrolytic cell is 0.5V-10.0V, an anode current density range is 0.05 A/cm 2 -1.50 A/cm 2 , and a cathode current density range is 0.05 A/cm 2 - 1.50 A/cm 2 .

6. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the electrolyte used in the electrolysis in the step S3 is a salt mixture composed of one or more of CsCl 2 , CaCl 2 , LiCl, NaCl, KCl, MgCl 2 , AlCl 3 , CaF, NaF, KF, and LiF and one or more of TiCl 3 , TiCl 2 , K 2 TiF 6 , and Na 2 TiF 6 .

7. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 6 , wherein a mass percent of titanium ions in the electrolyte is 1%-10%.

8. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the titanium-containing material is one or more of titanium dioxide, anatase type titanium white, titanium concentrate, titanium nitride, titanium carbide, titanium-carbon oxides, titanium-carbon-nitrogen oxides, metatitanic acid, ilmenite, vanadium titano-magnetite, blast furnace type high titanium slag, high titanium slag and titanium suboxides.

9. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the carbon-containing reducer is one or more of carbon, activated carbon, graphite powder, charcoal, petroleum coke, bitumen, and coal char particles.

10. The method for preparing metallic titanium by anode-electrolysis of carbonized/sulfurized ilmenite according to claim 1 , wherein the cathode is one or more of metallic titanium, stainless steel, carbon steel, metallic molybdenum and metallic nickel.

Assignees

• Univ Beijing Science & Technology

Inventors

• Jiao Shuqiang
• Tian Donghua
• Jiao Handong

Classifications

• B22F9/20

  starting from solid metal compounds · CPC title

• B22F2999/00

  Aspects linked to processes or compositions used in powder metallurgy · CPC title

• C25C7/025

  used in cells for the electrolysis of melts · CPC title

• C23C8/08

  only one element being applied · CPC title

• Y02P10/20

  Recycling · CPC title