Ultra high purity magnesium vacuum distillation purification met

Specialized metallurgical processes – compositions for use therei – Processes – Process control responsive to sensed condition

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75 1033, 75595, C22B 2622

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active

055826300

ABSTRACT:
Ultra high purity materials, particularly metallic materials such as magnesium and similarly high volatility materials, are produced by a vacuum distillation method and apparatus to increase purity by approximately five hundred times in a single step. For example, magnesium purity, exclusive of zinc content, is increased from 99.95% to greater than 99.9999%. A distillation column is formed of a high purity (less than 10 ppm ash) graphite, and includes a crucible, a vertical condenser in which horizontal high purity graphite baffles are selectively located at a plurality of levels, for example at nine levels. The column is contained in a three-zone resistance furnace that is controlled to heat the crucible to evaporate the material, maintain the condenser immediately above the crucible to above the boiling point of the material, and maintain the portion of the column thereabove at below the boiling point of the material, preferably with the temperature gradually decreasing with the height of the column. The baffles are spaced along the condenser and are staggered to slow the vapors such that the high purity material reaches its condensation temperature and condenses on one or more selected ones of the baffles. The condenser is split so the baffles can be selectively placed and removed to remove the purified material. Caps at the top and bottom of the column hold the split condenser together.

REFERENCES:
patent: 3767381 (1973-10-01), Bielefeldt
"Purification of Magnesium by Vacuum Distillation" by G. Revel, et al., 1978 The American Society For Metals And The Metallurgical Society of AIME, Metallurgic Transactions B, vol. 9B, Dec. 1978, pp. 665-672.
"Purification du magnesium par distillation sous vide"; or Purification of Magnesium by Vacuum Distallation by G. Revel, et al., Cent. Etud. Chim, Metall.; Vitry-sur-Seine, France; C. R. Hebd. Seances Acad. Sci. Paris, t281, 22 Dec. 1975, Serie C, pp. 1065-1068.
"Noveau magnesium de haute purete obtenu par zone fondue" or New High-Purity Magnesium Produced by Zone Melting, by Chaudron, Thierry; Revel, Gilles; Memoires Scientifiques Rev. Metallurg., vol. 64, No. 6, 1967, pp. 561-566.
"The Refining of Magnesium", The Refining of Non-Ferrous Metals, by E. F. Emley, The Institution of Mining and Metallurgy, London, 1950, pp. 407-443.
"Furnace for Refining of Magnesium" by O. Wallevik and J. B. Ronhaug; Extractive Metallurgy, Developments Since 1980, assigned to Norsk Hydro AS, Norway, Abstract of U.S. Patent No. 4,385,931, May 31, 1983.
Patent Abstracts of Japan, vol. 008 No. 067 (C-216), 29 Mar. 1984 & JP, A, 221242 (Nippon Jukagaku Kogypo KK) 22 Dec. 1983.

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