# US 2018/0023208 A1 · System and method for extraction and refining of titanium

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- Number: US 2018/0023208 A1
- Document ID: US20180023208A1
- Status: Published application
- Kind: A1
- Application number: 15/721,422
- Filed: 2017-09-29
- Published: 2018-01-25
- Earliest claimed: 2011-12-22
- Assignees: Universal Technical Resource Services, Inc.
- Applicants: Universal Technical Resource Services, Inc.
- Inventors: JAMES R. COX; CHANAKA L. DEALWIS; BENJAMIN A. KOHLER; MICHAEL G. LEWIS
- Web page: https://patentgrep.com/patent/US20180023208A1

## CPC

- C25C 3/28: of titanium
- C22B 34/1263: {obtaining metallic titanium from titanium compounds, e.g. by reduction (C22B34/129 takes precedence)}
- C22B 34/1277: {using other metals, e.g. Al, Si, Mn}
- C22C 14/00: Alloys based on titanium
- Y02P 10/20: Recycling
- C25C: PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- C22C: ALLOYS (treatment of alloys C21D, C22F)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A method to extract and refine metal products from metal-bearing ores, including a method to extract and refine titanium products. Titanium products can be extracted from titanium-bearing ores with TiO2 and impurity levels unsuitable for conventional methods.

## Claims

### Claim 1

A method for the production of titanium metal, comprising:
(a) heating a chemical blend to a temperature of between 1650° C.-1800° C., wherein the chemical blend comprises:
a titanium-bearing ore, comprising titanium oxide (TiO2);
an aluminum (Al) reducing agent, configured to reduce the titanium-bearing ore to a titanium product; and
a calcium fluoride (CaF2) viscosity agent,
wherein the chemical blend comprises a weight ratio of titanium oxide in the titanium-bearing ore to the aluminum (Al) in the aluminum reducing agent of between 0.9 to 2.4,
to form reaction products comprising:
(1) a titanium product, and (2) a residual slag;
(b) separating the residual slag from the titanium product;
(c) configuring the titanium product as an anode in an electrolytic cell, wherein the electrolytic cell is configured with an electrolyte consisting essentially of halide salts of alkali metals, halide salts of alkali earth metals, or combinations thereof;
(d) heating the electrolyte to a temperature between 600° C. and 900° C. to provide a molten electrolyte, wherein the molten electrolyte is in contact with the anode and a cathode;
(e) refining the titanium product by directing a current from the anode, through the molten electrolyte bath to the cathode to deposit a refined titanium product on the cathode; and
(f) recovering the refined titanium product, wherein the refined titanium product comprises at least 90 wt. % titanium.

### Claim 2 (depends on 1)

The method of claim 1, wherein the ratio of the titanium oxide component in the titanium-bearing ore to the aluminum (Al) component in the aluminum reducing agent to the calcium fluoride (CaF2) viscosity agent corresponds to a ratio of:
3 moles of titanium oxide, to
from 4 moles to not greater than 7 moles of aluminum (Al) reducing agent, to
from 2 moles to not greater than 6 moles of calcium fluoride (CaF2) viscosity agent.

### Claim 3 (depends on 1)

The method of claim 1, wherein the titanium bearing ore comprises ≦75% titanium oxide (TiO2) by weight.

### Claim 4 (depends on 1)

The method of claim 1, wherein the titanium-bearing ore comprises ≦50% titanium oxide (TiO2) by weight.

### Claim 5 (depends on 1)

The method of claim 1, wherein the step of heating the chemical blend further comprises: heating the chemical blend at a ramp up rate between 1° C. to 10° C./min.

### Claim 6 (depends on 1)

The method of claim 1, wherein the step of heating the chemical blend further comprises: heating the chemical blend at a ramp up rate between 1° C. to 50° C./min.

### Claim 7 (depends on 1)

The method of claim 1, wherein the step of heating the chemical blend further comprises: maintaining the chemical blend at 1650° C.-1800° C. for between 5 and 30 minutes.

### Claim 8 (depends on 1)

The method of claim 1, wherein the step of heating the chemical blend further comprises: maintaining the chemical blend at a temperature not less than 1700° C. for between 10 and 20 minutes.

### Claim 9 (depends on 1)

The method of claim 1, wherein the method comprises, prior to the configuring step, cooling the titanium product to a temperature less than 1670° C.

### Claim 10 (depends on 1)

The method of claim 1, wherein the titanium-bearing ore further comprises at least one of:
up to 20% calcium oxide (CaO),
up to 27% magnesium oxide (MgO),
up to 2% manganese oxide (MnO2), and
up to 46% iron oxide(s) (FeO and/or Fe2O3).

### Claim 11 (depends on 1)

The method of claim 1, wherein the ratio of titanium-bearing ore to aluminum (Al) reducing agent to calcium fluoride (CaF2) viscosity agent corresponds to the following equation:
3TiO2+(4+x)Al+yCaF2→3Ti+xAl+2Al2O3+yCaF2, and
wherein 0<x<3 and 2<y<6.

### Claim 12 (depends on 11)

The method of claim 11, wherein −0.3<x<2.

### Claim 13 (depends on 11)

The method of claim 11, wherein x=0.8 and y=2.5.

### Claim 14 (depends on 11)

The method of claim 11, wherein 0.3<x<2 and 2<y<3.

### Claim 15 (depends on 11)

The method of claim 11, wherein x=0.3 and y=2.0.

### Claim 16 (depends on 1)

The method of claim 1, wherein the titanium product comprises 28% to 94% titanium by weight with a yield of at least 85%.

### Claim 17 (depends on 1)

The method of claim 1, wherein the titanium product comprises at least 77% titanium by weight with a yield of at least 85% and up to 19% aluminum.

### Claim 18 (depends on 1)

The method of claim 1, wherein the anode is configured to include:
a mesh container and
the titanium product, and wherein the mesh container is non-consumable and the titanium product is retained in the mesh container and is consumable during the refining step.

### Claim 19 (depends on 18)

The method of claim 18, wherein the anode further includes at least one of: off-grade titanium metal, off-grade titanium sponge, or scrap titanium.

### Claim 20 (depends on 1)

The method of claim 1, wherein the refining step further comprises adjusting the anode such that the anode to cathode distance is between 1 cm and 6 cm.

### Claim 21 (depends on 1)

The method of claim 1, wherein heating the chemical blend is accomplished with an induction furnace.

### Claim 22

A method for the production of titanium metal, comprising:
(a) externally heating a chemical blend to a temperature of between 1500° C.-1600° C. to initiate an extraction reaction,
(b) subsequently elevating and maintaining the temperature at 1650° C.-1800° C. for between 5 and 30 minutes,
wherein the chemical blend comprises: a titanium-bearing ore comprising titanium oxide (TiO2), an aluminum (Al) reducing agent; and a calcium fluoride (CaF2) viscosity agent, and wherein the chemical blend comprises a ratio of the titanium-bearing ore to the aluminum (Al) reducing agent that corresponds to a weight ratio of titanium oxide component in the titanium-bearing ore to aluminum (Al) in the reducing agent of 0.9 to 2.4, and
wherein the extraction reaction results in the formation of (1) a titanium product, and (2) a residual slag;
(c) separating the residual slag from the titanium product; and
(d) refining the titanium product obtained from the extraction reaction in an electrochemical separation process comprising:
1. heating an electrolyte consisting of halide salts of alkali metals, halide salts of alkali earth metals, or combinations thereof to a temperature between 600° C. and 900° C. to provide a molten electrolyte;
2. configuring an anode and cathode in contact with said electrolyte wherein the anode comprises the titanium product;
3. applying an electrical differential between said anode and said cathode to deposit titanium on the cathode; and
4. recovering a refined titanium product.

### Claim 23 (depends on 22)

The method of claim 22, wherein the ratio of the titanium oxide to the aluminum (Al) reducing agent to the calcium fluoride (CaF2) viscosity agent corresponds to a ratio of:
3 moles of titanium oxide (TiO2) to
from 4 moles to not greater than 7 moles of the aluminum (Al) reducing agent, to
from 2 moles to not greater than 6 moles of the calcium fluoride (CaF2) viscosity agent.

### Claim 24 (depends on 22)

The method of claim 22, wherein the step of heating the chemical blend further comprises: heating the chemical blend at a ramp up rate of between 1° C. to 10° C./min.

### Claim 25 (depends on 22)

The method of claim 22, wherein the step of heating the chemical blend further comprises: heating the chemical blend at a ramp up rate between 1° C. to 50° C./min.

### Claim 26 (depends on 22)

The method of claim 22, wherein the step of heating the chemical blend further comprises: maintaining the chemical blend at a temperature not less than 1700° C. for between 10 and 20 minutes.

### Claim 27 (depends on 22)

The method of claim 22, further comprises, prior to the refining step, cooling the titanium product to a temperature less than 1670° C.

### Claim 28 (depends on 22)

The method of claim 22, wherein the titanium-bearing ore comprises 50% titanium oxide (TiO2) by weight.

### Claim 29 (depends on 22)

The method of claim 22, wherein the titanium-bearing ore further comprises at least one of:
up to 20% calcium oxide (CAO),
up to 27% magnesium oxide (MgO),
up to 11% silicon oxide (SiO2), and
up to 46% iron oxide (FeO or Fe2O3).

### Claim 30 (depends on 22)

The method of claim 22,
wherein the ratio of titanium-bearing ore to aluminum (Al) reducing agent to calcium fluoride (CaF2) viscosity agent corresponds to the following equation:
3TiO2+(4+x)Al+yCaF2→3Ti+xAl+2Al2O3+yCaF2, and
wherein 0<x<3 and 2<y<6.

### Claim 31 (depends on 30)

The method of claim 30, wherein 0.3<x<2 and 2<y<3.

### Claim 32 (depends on 30)

The method of claim 30, wherein x=0.8 and y=2.5.

### Claim 33 (depends on 30)

The method of claim 30, wherein x=0.3 and y=2.0.

### Claim 34 (depends on 22)

The method of claim 22, wherein the anode includes:
a mesh container and
the titanium product, and wherein the mesh container is non-consumable and the titanium product is retained in the mesh container and is consumable during the refining step.

### Claim 35 (depends on 34)

The method of claim 34, wherein the anode further includes at least one of: off-grade titanium metal, off-grade titanium sponge, or scrap titanium.

### Claim 36 (depends on 22)

The method of claim 22, wherein the electrical differential is between 1.0 volts and 1.8 volts.

### Claim 37 (depends on 22)

The method of claim 22, wherein the refining step further comprises configuring the anode such that the anode to cathode distance is between 1 cm and 6 cm.

### Claim 38

A method for the production of titanium metal, comprising:
(a) applying a thermal extraction process to a titanium-bearing ore, wherein the thermal extraction process comprises:
heating a chemical blend to a temperature of between 1500° C. and 1600° C., thereafter achieving and maintaining a temperature of between 1650° C. and 1800° C. for between 8 and 30 minutes, wherein the chemical blend comprises: a titanium-bearing ore comprising titanium oxide (TiO2); an aluminum (Al) reducing agent; and a calcium fluoride (CaF2) viscosity agent;
wherein the ratio of the titanium-bearing ore to the aluminum (Al) reducing agent to the calcium fluoride (CaF2) viscosity agent corresponds to a ratio of:
3 moles of a titanium oxide component (TiO2) in the titanium-bearing ore, to
from 4 moles to not greater than 7 moles of the aluminum (Al) reducing agent, to
from 2 moles to not greater than 6 moles of the calcium fluoride (CaF2) viscosity agent,
wherein the chemical blend reacts to form: (1) a titanium product, and (2) a residual slag;
(b) refining the titanium product in an electrochemical separation process, wherein the electrochemical separation process comprises:
1. configuring an anode and a cathode in contact with an electrolyte, said electrolyte consisting essentially of halide salts of alkali metals, halide salts of alkali earth metals, or combinations thereof, and said anode comprising the titanium product;
2. heating said electrolyte to a temperature between 600° C. and 900° C. to provide a molten electrolyte;
3. applying an electrical differential between the anode and the cathode to deposit refined titanium on the cathode; and
4. recovering a refined titanium product, wherein the refined titanium product comprises at least 90 wt. % titanium.