GB833103A - Improvements in or relating to the separation of zirconium and hafnium compounds - Google Patents
Improvements in or relating to the separation of zirconium and hafnium compoundsInfo
- Publication number
- GB833103A GB833103A GB37197/57A GB3719757A GB833103A GB 833103 A GB833103 A GB 833103A GB 37197/57 A GB37197/57 A GB 37197/57A GB 3719757 A GB3719757 A GB 3719757A GB 833103 A GB833103 A GB 833103A
- Authority
- GB
- United Kingdom
- Prior art keywords
- hafnium
- column
- tetrachloride
- hot end
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title abstract 2
- 238000000926 separation method Methods 0.000 title abstract 2
- 229910052726 zirconium Inorganic materials 0.000 title abstract 2
- 150000002363 hafnium compounds Chemical class 0.000 title 1
- 239000007788 liquid Substances 0.000 abstract 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract 4
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical class Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 abstract 4
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 abstract 4
- 229910052735 hafnium Inorganic materials 0.000 abstract 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 abstract 3
- 229910052786 argon Inorganic materials 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 2
- 238000010992 reflux Methods 0.000 abstract 2
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000004508 fractional distillation Methods 0.000 abstract 1
- 150000004820 halides Chemical class 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract 1
- 229910052753 mercury Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
<PICT:0833103/III/1> Zirconium and hafnium tetrachlorides are separated from mixtures thereof by subjecting the mixture to fractional distillation in a fractionating zone, in which the temperature of the hot end of the zone is in the range 455 DEG to 520 DEG C., and the absolute pressure is not less than 97% or more than 103% of that indicated by the equation: <FORM:0833103/III/1> where Pmm Hg is the pressure in millimetres of mercury, and TK DEG is the absolute temperature of the hot end of the zone. The pressures corresponding to this formula range from 5.69 X 104 mm. Hg to 2.23 X 104 mm. Hg. Zirconium tetrachloride of reduced hafnium content is removed from the hot end, and enriched hafnium tetrachloride from the low temperature end. The process may be carried out in a column of at least 30 theoretical plates. The temperature at the hot end being between 460 DEG C. and 512 DEG C. and the still head above the column being cooled to not below 440 DEG C. to provide a liquid reflux, pure hafnium tetrachloride being recovered from the top of the column and pure zirconium tetrachloride from a lower part. In an example (illustrated by Fig. 2), an impure zirconium tetrachloride, containing 1.6% hafnium tetrachloride, was introduced into the boiler 24 in an argon atmosphere, and then argon was introduced into the whole system to a pressure of about 19,400 mm. Hg. The whole system was then heated, and the column 17 and boiler 29 were filled with halide vapour and some liquid, the argon being removed via valve 7. The pressure in the system was maintained at 28,180-28,440 mm. Hg by heating the boiler 29 by means of heater 33. The top of the column is maintained at about 440 DEG C., and a continuous separation may be achieved, pure zirconium tetrachloride being withdrawn either as liquid through 26 or as vapour through 30, and a fraction rich in hafnium collected in 14a or withdrawn via 14b. The condenser 8 provides a reflux liquid for the column, and the hafnium fraction is condensed by condenser 9. The whole apparatus is jacketed so that suitable temperature controlling liquids, such as molten salts, may be circulated.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US833103XA | 1956-12-07 | 1956-12-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB833103A true GB833103A (en) | 1960-04-21 |
Family
ID=22177499
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB37197/57A Expired GB833103A (en) | 1956-12-07 | 1957-11-28 | Improvements in or relating to the separation of zirconium and hafnium compounds |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB833103A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2150549A (en) * | 1983-12-01 | 1985-07-03 | Pavel Hurt | Process for the separate recovery of metal chlorides from complex ores etc |
-
1957
- 1957-11-28 GB GB37197/57A patent/GB833103A/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2150549A (en) * | 1983-12-01 | 1985-07-03 | Pavel Hurt | Process for the separate recovery of metal chlorides from complex ores etc |
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