US3859077A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Manufacture of titanium chloride, synthetic rutile and metallic iron from titaniferous materials containing iron
Assignee: Individual
•
Filing: 1973-04-20
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Granted: 1975-01-07
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Expires: 1993-04-20
Abstract
Abstract Substantially pure titanium dioxide is made under reducing conditions by a halogen-oxygen interchange between a titanium tetrahalide and an oxide of iron contained in a slag, or an ore such as ilmenite, at a temperature, approximately 1000*C. The iron and some impurities such as phosphorus, sulfur, vanadium, and chromium are volatilized as halides or oxyhalides. Solid titanium dioxide remains with some impurities which may be washed out with water or an aqueous acid or alkali. The gaseous ferrous halide is then reacted with some or all of the titanium dioxide and a reductant at a temperature above about 1550*C so as to be reduced to molten metallic iron and to give the gaseous titanium halide which is passed to the first reactor. Only makeup halogen is required.
Inventors
- 👤 Donald F Othmer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 11:07
CPC Classifications
C; C22; C22B; C22B34/00; C22B34/10; C22B34/12; C22B34/1218; C22B34/1222; C21; C21B; C21B15/00; C21B15/006; C22B34/1204; C22B34/1209; Y; Y02; Y02P; Y02P10/00; Y02P10/20
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
208 words
A PROCESS CONDUCTED AT APPROXIMATELY ATMOSPHERIC PRESSURE FOR MAKING METALLIC IRON IN A DENSE PHASE FROM AN ORIGINAL MATIERAL IN THE FORM OF PARTICULATE SOLIDS CONTAINING TITANIUM OXIDE AND IRON OXIDE SAID PROCESS COMPRISING THE STEPS OF: A. PASSING SAID ORIGINAL MATERIAL INTO A FIRST REACTION ZONE WHEREIN, AT A TEMPERATURE BETWEEN ABOUT 950*C AND 1100*C IN THE PRESENCE OF A CARBONACEOUS REDUCTANT, A TITANIUM HALIDE IN AN ADDED GASEOUS STREAM HALOGENATES IN A FIRST CHEMICAL REACTION A SUBSTANTIAL PART OF THE IRON IN SAID IRON OXIDE IN SAID ORIGINAL MATERIAL TO PRODUCE AN IRON HALIDE IN SAID GAS STREAM AND ADDITIONAL TITANIUM OXIDE; B. SEPARATING SAID GAS STREAM CONTAINING SAID IRON HALIDE FROM THE SOLID RESIDUE OF SAID FIRST CHEMICAL REACTION, SAID SOLID RESIDUE CONTAINING BOTH SAID TITANIUM OXIDE IN SAID ORIGINAL MATERIAL AND SAID ADDITIONAL TITANIUM OXIDE PRODUCED IN SAID FIRST CHEMICAL REACTION AND HAVING A GREATER RATIO OF ATOMS OF TITANIUM TO ATOMS OF IRON THAN THIS RATIO IN SAID ORIGINAL MATERIAL; C. PASSING SAID SEPARATED GAS STREAM CONTAINING SAID IRON HALIDE INTO A SECOND REACTION ZONE MAINTAINED AT A TEMPERATURE BETWEEN 1100*C AND ABOUT 1800*C; D. PASSING AT LEAST A PART OF SAID SOLID RESIDUE CONTAINING SAID TITANIUM DIOXIDE INTO SAID SECOND REACTION ZONE;
Claim 2
Dependent Claim
208 words
A PROCESS CONDUCTED AT APPROXIMATELY ATMOSPHERIC PRESSURE FOR MAKING METALLIC IRON IN A DENSE PHASE FROM AN ORIGINAL MATIERAL IN THE FORM OF PARTICULATE SOLIDS CONTAINING TITANIUM OXIDE AND IRON OXIDE SAID PROCESS COMPRISING THE STEPS OF: A. PASSING SAID ORIGINAL MATERIAL INTO A FIRST REACTION ZONE WHEREIN, AT A TEMPERATURE BETWEEN ABOUT 950*C AND 1100*C IN THE PRESENCE OF A CARBONACEOUS REDUCTANT, A TITANIUM HALIDE IN AN ADDED GASEOUS STREAM HALOGENATES IN A FIRST CHEMICAL REACTION A SUBSTANTIAL PART OF THE IRON IN SAID IRON OXIDE IN SAID ORIGINAL MATERIAL TO PRODUCE AN IRON HALIDE IN SAID GAS STREAM AND ADDITIONAL TITANIUM OXIDE; B. SEPARATING SAID GAS STREAM CONTAINING SAID IRON HALIDE FROM THE SOLID RESIDUE OF SAID FIRST CHEMICAL REACTION, SAID SOLID RESIDUE CONTAINING BOTH SAID TITANIUM OXIDE IN SAID ORIGINAL MATERIAL AND SAID ADDITIONAL TITANIUM OXIDE PRODUCED IN SAID FIRST CHEMICAL REACTION AND HAVING A GREATER RATIO OF ATOMS OF TITANIUM TO ATOMS OF IRON THAN THIS RATIO IN SAID ORIGINAL MATERIAL; C. PASSING SAID SEPARATED GAS STREAM CONTAINING SAID IRON HALIDE INTO A SECOND REACTION ZONE MAINTAINED AT A TEMPERATURE BETWEEN 1100*C AND ABOUT 1800*C; D. PASSING AT LEAST A PART OF SAID SOLID RESIDUE CONTAINING SAID TITANIUM DIOXIDE INTO SAID SECOND REACTION ZONE;
Claim 3
Dependent Claim
29 words
The process according to claim 1 wherein the temperature in said second reaction zone is above 1535*C and said metallic iron is formed and removed in the liquid state.
Claim 4
Dependent Claim
43 words
The process according to claim 1 wherein at least a part of said solid residue produced by said first reaction and having a higher ratio of atoms of titanium to atoms of iron than in said original material is removed as a product.
Claim 5
Dependent Claim
47 words
The process according to claim 1 wherein at least a part of said titanium halide coming in a gas stream from said second chemical reaction is removed as a product, having a higher ratio of atoms of titanium to atoms of iron than in said original material.
Claim 6
Dependent Claim
44 words
The process according to claim 1 wherein said gas stream containing titanium halide formed in said second chemical reaction is separated from at least a part of the materials other than said titanium halide it contains before being utilized in said first chemical reaction.
Claim 7
Dependent Claim
24 words
The process according to claim 1 wherein said titanium halide is titanium tetrachloride, and said iron halide is, at least in part, ferrous chloride.
Claim 8
Dependent Claim
91 words
The process according to claim 6 wherein: a. said ferrous chloride is produced in said first chemical reaction as a gaseous stream which is separated from said solid residue having a higher ratio of atoms of titanium to atoms of iron than in said original material; b. said gaseous stream containing said ferrous chloride, and said solid residue containing said titanium oxide are passed to said second chemical reaction wherein said ferrous chloride and said titanium oxide in said solid residue are contacted in counter-current and reacted chemically with each other.
Claim 9
Dependent Claim
66 words
The process according to claim 7 wherein said gaseous stream separated from said solid residue from said first chemical reaction contains other gases in additIon to said ferrous chloride; and at least some part of said other gases is removed from said stream; and said ferrous chloride in a more pure form than it left said first chemical reaction is passed to said second chemical reaction.
Claim 10
Dependent Claim
110 words
The process according to claim 6 wherein said first chemical reaction is accomplished during a first concurrent flow and contacting of a mixture of the particulate solids comprising said original material and said solid reductant, with a gas phase which contains a gas capable of chlorinating at least one of the constituents of said original material; and said second chemical reaction is accomplished at the higher temperature during a second concurrent flow of solids resulting from said first chemical reaction and the gas phase resulting from said first chemical reaction, which gas phase contains a gas capable of chlorination of at least one of the constituents of said original material.
Claim 11
Dependent Claim
28 words
The process according to claim 9 wherein said gas phase at the discharge of said concurrent contacting during which said second chemical reaction is accomplished contains titanium tetrachloride.
Claim 12
Dependent Claim
53 words
The process according to claim 10 wherein said discharging gas containing titanium tetrachloride has at least a part of the other materials also contained therein removed; and the remaining of said titanium tetrachloride is recycled, at least in part, to the beginning of said concurrent contacting wherein said first chemical reaction is accomplished.
Claim 13
Dependent Claim
71 words
The process according to claim 9 wherein said first concurrent contacting accomplishes sequentially said first chemical reaction, and said second concurrent flow accomplishes said second chemical reaction, while feeding said original material and gaseous chlorine into the top of a single reactor vessel having said first reaction zone above said second reaction zone and discharging titanium tetrachloride in a gas stream and molten iron from the bottom of said reactor vessel.
Claim 14
Dependent Claim
80 words
The process according to claim 11 wherein: a. at least a part of said gaseous titanium tetrachloride, a reactant for said first chemical reaction, is produced by the preliminary reaction of gaseous chlorine with the titanium oxide in said original material in the presence of said carbonaceous reductant; b. said products of said preliminary reaction continue said concurrent flow and concurrent contacting throughtout the respective zones wherein said first chemical reaction takes place and said second chemical reaction takes place.
Claim 15
Dependent Claim
34 words
The process according to claim 6 wherein said first chemical reaction is accomplished in a counter-current contacting of the particulate solids of said original material and said solid reductant with said gaseous titanium tetrachloride.
Claim 16
Dependent Claim
49 words
The process according to claim 6 wherein said second chemical reaction is accomplished in a counter-current contacting of at least a part of said titanium oxide in said solid residue of said first chemical reaction with said ferrous chloride in gaseous form also produced by said first chemical reaction.
Claim 17
Dependent Claim
52 words
The process according to claim 1 wherein the solids resulting from said first chemical raction with said original material and then second chemical reaction starting with said residue of said first chemical reaction are heated to a final maximum temperature, above the melting point of iron, without an intermediary cooling and reheating.
Claim 18
Dependent Claim
59 words
The process according to claim 16 wherein at least some part of the heat required to bring the reactants of at least one of the two said chemical reactions up to its respective optimum temperature is supplied by the combustion of said carbonaceous reductant through the addition of an oxygen-containing gas to at least one of said reaction zones.
Claim 19
Dependent Claim
58 words
The process according to claim 4 wherein: said titanium halide is titanium tetrachloride; said iron halide is, at least in part, ferrous chloride; and chlorine gas is supplied to at least one of the two said chemical reactions in a total amount at least stOichiometrically equivalent to that in said titanium tetrachloride which is removed as a product.
Claim 20
Dependent Claim
40 words
The process according to claim 18 wherein said chlorine gas is supplied in amount sufficient to form chlorine compounds with at least some of the metals present as compounds in said original material other than compounds of titanium and iron.
Claim 21
Dependent Claim
51 words
The process according to claim 19 wherein at least some of said chlorine compounds of metals present as compounds in said original material other than compounds of titanium and iron are more volatile than ferrous chloride and are separated from the gaseous stream of ferrous chloride leaving said first chemical reaction.
Claim 22
Dependent Claim
50 words
The process according to claim 19 wherein at least some of said chlorine compounds of metals present as compounds in said original material other than compounds of titanium and iron are more volatile than ferrous chloride and are separated from the gaseous titanium tetrachloride formed in said second chemical reaction.
Claim 23
Dependent Claim
48 words
The process according to claim 19 wherein at least some of said chlorine compounds of metals present as compounds in said original material other than compounds of titanium and iron are less volatile than ferrous chloride and are separated from said solid residue of said first chemical reaction.
Claim 24
Dependent Claim
53 words
The process according to claim 6 wherein at least a part of said titanium oxide in said solid residue of said first chemical reaction is withdrawn after said first chemical reaction as a product containing a greater ratio of atoms of titanium to atoms of iron than this ratio in said original material.
Claim 25
Dependent Claim
72 words
The process according to claim 20 wherein at least some of said chlorine compounds of metals present as compounds in said original material other than compounds of titanium and iron are less volatile than ferrous chloride and are separated from said solid residue of said first chemical reaction; and at least a part of said gas stream leaving said second chemical reaction is removed as a product containing substantially pure titanium tetrachloride.
Claim 26
Dependent Claim
12 words
The process according to claim 6 wherein said original material is ilmenite.
Claim 27
Dependent Claim
42 words
The process according to claim 6 wherein said carbonaceous reductant present in said second chemical reaction was added to and was present during said first chemical reaction from which it was discharged in said solid residue passed to said second chemical reaction.
Claim 28
Dependent Claim
15 words
The process according to claim 6 wherein the several steps are conducted in batch processing.
Claim 29
Dependent Claim
39 words
The process according to claim 6 wherein said first chemical reaction and said second chemical reaction are conducted in continuous gas-solid counter-current contacting reactors, at least one of which has from one to three equilibrium units of contacting efficiency.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-01-06 | 1978-07-08 | 1979-01-07 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-01-06 | 1982-07-08 | 1983-01-07 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-01-06 | 1986-07-08 | 1987-01-07 | $7700.00 | Window Closed / Lapsed |