US2519385A - Production of titanium tetraiodide - Google Patents

Production of titanium tetraiodide Download PDF

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Publication number
US2519385A
US2519385A US20595A US2059548A US2519385A US 2519385 A US2519385 A US 2519385A US 20595 A US20595 A US 20595A US 2059548 A US2059548 A US 2059548A US 2519385 A US2519385 A US 2519385A
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United States
Prior art keywords
titanium
tetraiodide
iodine
titanium tetrachloride
tetrachloride
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Expired - Lifetime
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US20595A
Inventor
Alfred C Loonam
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Chilean Nitrate Corp
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Chilean Nitrate Corp
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Priority to US20595A priority Critical patent/US2519385A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium

Definitions

  • This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide.
  • metallic titanium of high purity is produced by contacting titanium tetraiodide with a heated surface maintained at a temperature in the range 1100 C. to 1700" C.
  • Contact of the titanium tetraiodide with the heated surface results in dissociation of the iodine and titanium of the titanium tetraiodide with the deposition of the titanium on the heated surface and with the production of a gaseous product containing the iodine in vapor form.
  • Titanium or tungsten or some other suitable metal is employed in forming the heated surface.
  • the titanium tetraiodide employed is formed by contacting iodine in vapor form with crude metallic titanium.
  • titanium tetraiodide is produced by contacting elemental iodine in vapor form with titanium carbide.
  • the production of titanium tetraiodide by reaction of iodine in vapor form with titanium carbide is described and claimed in my co-pending applications, Serial Nos. 20,593, and 20,598, both filed April 12, 1948.
  • the elemental iodine in vapor form is contacted with the titanium carbide at a temperature near 1100 C.
  • the present invention is based on my discovery that the reaction between elemental iodine in vapor form and titanium carbide is accelerated and may be carried out at a lower temperature if carried out in the presence of a small amount of titanium tetrachloride. In the presence of titanium tetrachloride, the reaction proceeds at least as rapidly at 1600 C. as it does at 1100" C. in the absence of titanium tetrachloride.
  • the iodine and titanium tetrachloride may be employed in any desired proportions, but a mixture of iodine and titanium tetrachloride in which the titanium tetrachloride is present in amount by weight equal to about one to five percent (l.% to 5%) of the weight of the iodine will produce satisfactory results.
  • the gaseous product resulting from treatment of the titanium carbide with iodine in the presence of titanium tetrachloride contains titanium tetraiodide and titanium tetrachloride. Excess iodine may be present, also, in the gaseous product resulting from the treatment of titanium carbide with iodine.
  • the boiling point of titanium tetrachloride is 136x? C.
  • the boiling point of titanium tetraiodide is 379 C.
  • Quantitative separation of the two compounds can be effected by means of a suitable fractionating treatment as, for example, by fractional condensation of the gaseous products or by complete condensation of the gaseous product followed by fractional distillation.
  • the separated titanium tetrachloride may be returned to the process for re-use.
  • the iodine and the titanium tetrachloride present in the gaseous product may be separated together and returned together to the process for re-use in treating titanium carbide.
  • the method of preparing titanium tetraiodide which comprises heating titanium carbide with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride.
  • the method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride.
  • the method of preparing titanium tetraiodide which comprises heating titanium carbide 3 with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, and i'ractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products.
  • the method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, and fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products.
  • the method of preparing titanium tetraiodide which comprises heating titanium carbide with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products, and returning the titanium tetrachloride to the process for re-use.
  • the method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products, and returning the titanium tetrachloride to the process for re-use.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Description

Patented Aug. 22, 1950 UNITED STATES PATENT OFFICE PRODUCTION OF TITANIUM TETRAIODIDE No Drawing. Application April 12, 1948, Serial No. 20,595
6 Claims.
This invention relates to the production of metallic titanium and has for an object the provision of an improved method or process for producing high-purity metallic titanium. More particularly, the invention contemplates the provision of an improved method or process for producing high-purity metallic titanium by dissociation of titanium tetraiodide.
According to some heretofore customary procedures, metallic titanium of high purity is produced by contacting titanium tetraiodide with a heated surface maintained at a temperature in the range 1100 C. to 1700" C. Contact of the titanium tetraiodide with the heated surface results in dissociation of the iodine and titanium of the titanium tetraiodide with the deposition of the titanium on the heated surface and with the production of a gaseous product containing the iodine in vapor form. Titanium or tungsten or some other suitable metal is employed in forming the heated surface.
According to some heretofore customary processes, the titanium tetraiodide employed is formed by contacting iodine in vapor form with crude metallic titanium.
According to the process of my invention, titanium tetraiodide is produced by contacting elemental iodine in vapor form with titanium carbide. The production of titanium tetraiodide by reaction of iodine in vapor form with titanium carbide is described and claimed in my co-pending applications, Serial Nos. 20,593, and 20,598, both filed April 12, 1948.
In the production of titanium tetraiodide by reaction of iodine with titanium carbide, as de' scribed in my aforementioned co-pending applications, the elemental iodine in vapor form is contacted with the titanium carbide at a temperature near 1100 C.
The present invention is based on my discovery that the reaction between elemental iodine in vapor form and titanium carbide is accelerated and may be carried out at a lower temperature if carried out in the presence of a small amount of titanium tetrachloride. In the presence of titanium tetrachloride, the reaction proceeds at least as rapidly at 1600 C. as it does at 1100" C. in the absence of titanium tetrachloride.
The iodine and titanium tetrachloride may be employed in any desired proportions, but a mixture of iodine and titanium tetrachloride in which the titanium tetrachloride is present in amount by weight equal to about one to five percent (l.% to 5%) of the weight of the iodine will produce satisfactory results.
The titanium tetrachloride functions somewhat in the manner of a catalyst in accordance with reactions illustrated by the following equations:
The gaseous product resulting from treatment of the titanium carbide with iodine in the presence of titanium tetrachloride contains titanium tetraiodide and titanium tetrachloride. Excess iodine may be present, also, in the gaseous product resulting from the treatment of titanium carbide with iodine. The boiling point of titanium tetrachloride is 136x? C. The boiling point of titanium tetraiodide is 379 C. Quantitative separation of the two compounds can be effected by means of a suitable fractionating treatment as, for example, by fractional condensation of the gaseous products or by complete condensation of the gaseous product followed by fractional distillation. The separated titanium tetrachloride may be returned to the process for re-use.
In the fractionation treatment, the iodine and the titanium tetrachloride present in the gaseous product may be separated together and returned together to the process for re-use in treating titanium carbide.
I claim:
1. The method of preparing titanium tetraiodide which comprises heating titanium carbide with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride.
2. The method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride.
3. The method of preparing titanium tetraiodide which comprises heating titanium carbide 3 with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, and i'ractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products.
4. The method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, and fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products.
5. The method of preparing titanium tetraiodide which comprises heating titanium carbide with iodine in vapor form in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products, and returning the titanium tetrachloride to the process for re-use.
6. The method of preparing titanium tetraiodide which comprises subjecting titanium carbide to the action of iodine in vapor form at a temperature of about 1000 C. in the presence of titanium tetrachloride to produce a gaseous product comprising titanium tetraiodide and titanium tetrachloride, fractionating the gaseous product to obtain separate titanium tetraiodide and titanium tetrachloride products, and returning the titanium tetrachloride to the process for re-use.
ALFRED C. LOONAM.
No references cited.

Claims (1)

  1. 3. THE METHOD OF PREPARING ITANIUM TETRAIODIDE WHICH COMPRISES HEATING TITANIUM CARBIDE WITH IODINE IN VAPOR FORM IN THE PRESENCE OF TITANIUM TETRACHLORIDE TO PRODUCE A GASEOUS PRODUCT COMPRISING TITANIUM TETRAIODIDE AND TITANIUM TETRACHLORIDE, AND FRACTIONATING THE GASEOUS PRODUCT TO OBAIN SEPARATE TITANIUM TETRAIODIDE AND TITANIUM TETRACHLORIDE PRODUCTS.
US20595A 1948-04-12 1948-04-12 Production of titanium tetraiodide Expired - Lifetime US2519385A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2694653A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694652A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2716051A (en) * 1953-11-13 1955-08-23 Ivor E Campbell Method of producing zirconium halide
US2770541A (en) * 1952-08-14 1956-11-13 Nat Res Corp Method of producing titanium
US2783142A (en) * 1952-08-14 1957-02-26 Nat Res Corp Method of producing titanium
US2868704A (en) * 1954-11-30 1959-01-13 Horizons Titanium Corp Production of lower valent halides of ta, nb, ti and v
US2876180A (en) * 1953-12-14 1959-03-03 Horizons Titanium Corp Fused salt bath for the electrodeposition of transition metals
US2907632A (en) * 1955-08-24 1959-10-06 Monsanto Chemicals Production of titanium tetraiodide
US2940825A (en) * 1954-11-26 1960-06-14 Monsanto Chemicals Method for producing titanium trichloride
WO2016089953A1 (en) * 2014-12-05 2016-06-09 Moog Inc. Neutralization of reactive metal condensate in additive manufacturing

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2694653A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2694652A (en) * 1948-04-12 1954-11-16 Chilean Nitrate Sales Corp Production of metallic titanium
US2770541A (en) * 1952-08-14 1956-11-13 Nat Res Corp Method of producing titanium
US2783142A (en) * 1952-08-14 1957-02-26 Nat Res Corp Method of producing titanium
US2716051A (en) * 1953-11-13 1955-08-23 Ivor E Campbell Method of producing zirconium halide
US2876180A (en) * 1953-12-14 1959-03-03 Horizons Titanium Corp Fused salt bath for the electrodeposition of transition metals
US2940825A (en) * 1954-11-26 1960-06-14 Monsanto Chemicals Method for producing titanium trichloride
US2868704A (en) * 1954-11-30 1959-01-13 Horizons Titanium Corp Production of lower valent halides of ta, nb, ti and v
US2907632A (en) * 1955-08-24 1959-10-06 Monsanto Chemicals Production of titanium tetraiodide
WO2016089953A1 (en) * 2014-12-05 2016-06-09 Moog Inc. Neutralization of reactive metal condensate in additive manufacturing
CN107000120A (en) * 2014-12-05 2017-08-01 穆格公司 Neutralization of the reactive metal condensate in increasing material manufacturing

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