IP Library Granted Patent US 10,689,730
Granted Patent B2
US 10,689,730 · App. 14/935,245 · Granted Jun 23, 2020

Methods of producing a titanium product

Inventors: Zhigang Zak Fang (Salt Lake City, UT); Ying Zhang (Salt Lake City, UT); Yang Xia (Salt Lake City, UT); Pei Sun (Salt Lake City, UT)
Assignee: University of Utah Research Foundation
C22B7/04B22F9/20C01B6/02C22B1/02C22B3/04C22B34/1204C22B34/1213C22B34/1259C22B34/1268C22B34/1277C22B34/1286C22B34/1295B22F2201/013B22F2301/205
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Quick Facts
Patent No.
US 10,689,730
App. No.
14/935,245
Granted
Jun 23, 2020
Kind
B2
Abstract

A method ( 500 ) for producing a titanium product is disclosed. The method ( 500 ) can include obtaining TiO 2 -slag ( 501 ) and reducing impurities in the TiO 2 -slag ( 502 ) to form purified TiO 2 ( 503 ). The method ( 500 ) can also include reducing the purified TiO 2 using a metallic reducing agent ( 504 ) to form a hydrogenated titanium product comprising TiH 2 ( 505 ). The hydrogenated titanium product can be dehydrogenated ( 506 ) to form a titanium product ( 508 ). The titanium product can also be optionally deoxygenated ( 507 ) to reduce oxygen content.

Claims (39)

1. A method for producing a titanium product, comprising:

obtaining TiO 2 rich material as a purified TiO 2 having at least 70% by weight TiO 2 ;

reducing the purified TiO 2 by combining with a metallic reducing agent and a molten salt at a temperature and a pressure to produce a hydrogenated titanium powder product comprising TiH 2 and optionally elemental titanium;

heat treating the hydrogenated titanium powder product under a hydrogen atmosphere to coarsen the powder so as to reduce pore size and specific surface area to form a heat treated hydrogenated titanium powder product, wherein the hydrogen atmosphere is maintained during at least one of heating and cooling; and

deoxygenating the heat treated hydrogenated titanium powder product to reduce residual oxygen to less than 0.2 wt % to form a deoxygenated hydrogenated titanium powder product.

2. The method of claim 1 , further comprising reducing impurities in the TiO 2 rich material to produce the purified TiO 2 .

3. The method of claim 2 , wherein the TiO 2 rich material is a TiO 2 -slag having a TiO 2 content from 70 wt % to 90 wt %.

4. The method of claim 3 , wherein the UGS has a TiO 2 content greater than 90 wt %.

5. The method of claim 2 , wherein the TiO 2 rich material is upgraded TiO 2 -slag (UGS).

6. The method of claim 2 , wherein the reducing impurities includes alkaline roasting the TiO 2 rich material to remove impurities from the TiO 2 rich material and produce intermediate products including alkaline leached TiO 2 rich material.

7. The method of claim 6 , wherein alkaline roasting comprises:

combining NaOH with the TiO 2 rich material at a second temperature to transform TiO 2 into sodium titanate and to transform impurities into salts; and

washing the sodium titanate with water to remove the salts and produce derivatives of sodium titanate.

8. The method of claim 7 , wherein the second temperature is between about 450° C. and about 650° C.

9. The method of claim 7 , wherein the reducing impurities further comprises desilicating the alkaline roasted and water washed TiO 2 rich material to lower silica content prior to reducing.

10. The method of claim 9 , wherein the desilicating is accomplished using a silica gel and a flocculant.

11. The method of claim 2 , wherein the reducing impurities further comprises pre-leaching the TiO 2 rich material using an aqueous NaOH solution to remove silica.

12. The method of claim 2 , wherein the reducing impurities further comprises:

hydrolyzing the TiO 2 rich material to form a titanic acid; and

calcining the titanic acid to form a coarse purified TiO 2 as the purified TiO 2 .

13. The method of claim 12 , wherein the coarse purified TiO 2 has a specific surface area from 10 m 2 /g to 100 m 2 /g, and an average particle diameter from 1 μm to 100 μm.

14. The method of claim 1 , wherein the purified TiO 2 has greater than about 99 wt % TiO 2 .

15. The method of claim 1 , wherein the purified TiO 2 has greater than about 99.5 wt % TiO 2 .

16. The method of claim 1 , wherein the purified TiO 2 is purchased commercially.

17. The method of claim 1 , wherein the metallic reducing agent comprises at least one of Mg, MgH 2 , and CaH 2 .

18. The method of claim 1 , wherein the molten salt comprises at least one of a mono chloride, binary chloride salt and a ternary chloride salt.

19. The method of claim 1 , wherein the reducing occurs in a hydrogen atmosphere and the metallic reducing agent is Mg and MgH 2 .

20. The method of claim 1 , wherein the specific surface area of the heat treated hydrogenated titanium product is from about 0.01 m 2 /g to 0.5 m 2 /g.

21. The method of claim 1 , wherein the deoxygenating is accomplished by heating a molten calcium salt in the presence of solid calcium and the titanium product to a temperature below the melting point of calcium.

22. The method of claim 21 , wherein the molten calcium salt includes CaCl 2 and at least one of KCl and LiCl.

23. The method of claim 1 , wherein the method is free of chlorination and electrolysis.

24. The method of claim 1 , wherein the molten salt includes MgCl 2 .

25. The method of claim 1 , further comprising removing MgO from the hydrogenated titanium product prior to deoxygenating.

26. The method of claim 1 , wherein the deoxygenating is accomplished using CaH 2 .

27. The method of claim 1 , wherein the deoxygenating occurs under one or both of Argon and hydrogen atmosphere.

28. The method of claim 1 , further comprising leaching impurities including MgO from the deoxygenated hydrogenated titanium product.

29. The method of claim 1 , wherein the heat treating includes:

heating the hydrogenated titanium product where the hydrogen atmosphere is controlled to maintain a hydrogen content of the hydrogenated titanium product; or

heating the hydrogenated titanium product under an argon atmosphere and then switching to the hydrogen atmosphere during a cooling phase.

Assignments (3)
CONFIRMATORY LICENSE Recorded Jan 18, 2018
From: UNIVERSITY OF UTAH
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 045085/0564 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2016
From: FANG, ZHIGANG ZAK; ZHANG, YING; XIA, YANG; SUN, PEI
To: UNIVERSITY OF UTAH
Reel/Frame 038521/0784 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2016
From: UNIVERSITY OF UTAH
To: UNIVERSITY OF UTAH RESEARCH FOUNDATION
Reel/Frame 038521/0825 →
Continuity (3)
Continuation In Part PCTUS2014051621 · Aug 19, 2014
Provisional Application 61867467 · Aug 19, 2013
Related Publication 20160108497A1 · Apr 21, 2016