US2252052A - Sublimating apparatus - Google Patents

Sublimating apparatus Download PDF

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Publication number
US2252052A
US2252052A US298330A US29833039A US2252052A US 2252052 A US2252052 A US 2252052A US 298330 A US298330 A US 298330A US 29833039 A US29833039 A US 29833039A US 2252052 A US2252052 A US 2252052A
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United States
Prior art keywords
cover
temperature
sublimate
crucible
heat
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Expired - Lifetime
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US298330A
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English (en)
Inventor
Hendrik Johannes Meerka Embden
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Hartford National Bank and Trust Co
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Hartford National Bank and Trust Co
Priority date (The priority date 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 date listed.)
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Publication date
Application filed by Hartford National Bank and Trust Co filed Critical Hartford National Bank and Trust Co
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D7/00—Sublimation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B35/00—Obtaining beryllium

Definitions

  • My invention relates to an apparatus for sublimating materials under low pressure.
  • iodine and the light metals such as magnesium, beryllium and the like
  • the ores together with a reducing agent are placed in a suitable apparatus and are heated at a temperature of more than 1000 C. in an atmosphere of low pressure, for instance 2 cms. of mercury or less.
  • the metal is vaporized immediately by the high temperature and low pressure, and the vapors thereof pass to colder portions, i. e. condensing portions, of the apparatus and condense on the surface thereof to form a sublimate.
  • the sublimate will be in a very finely divided form. This has the disadvantage that when the apparatus is opened to remove the sublimate, the sublimate, due to its finely-divided state, will be readily oxidized by air. For this reason there will be losses due to oxidation and the sublimate may even be set on fire.
  • the object of my invention is to overcome the above difiiculties and for this purpose I provide an apparatus in which substantially all the heat removed from the condensing portion is transthereof will be maintained above that tempera- I ture at which the vapors condense crystallized form.
  • the apparatus of the invention ensures a very in a coarse exact regulation of the temperature of the condensing portion because any increase inits temperature caused by an increase in the amount of the sublimate being condensed thereon will be automatically compensated by an increase in the amount of heat radiated. Similarly, a decrease in the temperature will be compensated by a decrease in the radiation.
  • I provide a cooling jacket which has a surface opposing the surface of the condensing portion with a narrow intermediate space, which is evacuated. In this case the dissipation of heat from the condensing member to the cooling system is retarded and the condensing member gives off its heat only at higher temperatures.
  • the apparatus shown in the drawing comprises a crucible of a refractory non-conductive material which contains a charge 2.
  • the charge 2 includes the ore of the metal to be sublimated, a reducing agent, and, if it is non-conductive, also a conducting material.
  • the crucible I is supported on a base plate 5, of stoneware, and a vacuum-tight cylinder 6, for instance of porcelain, has its lower flanged end resting upon the plate 5 to form a hermeticallytight joint therewith.
  • the charge I is heated by a high-frequency field generated by a winding 8 surrounding the cylinder 6.
  • a double-walled cooling jacket 1 Resting upon the top flange of cylinder 8 so as to form a hermetically-tight joint therewith is a double-walled cooling jacket 1 provided on its upper end with a flanged tubular extension 15 forming an outlet l0.
  • the jacket 'I is located outside the high-frequency field generated by winding' 8 it may be made of metal.
  • The'jacket l is filled with water 9 to maintain its temperature low enough to prevent warping and to take up the heat produced by condensation of the vapor and radiated from the outer surface 3 of the cover [2 through space 4 to the opposing surface it of the jacket'l.
  • This jacket is provided with an outlet passage I8 for the removal of steam formed by the heating of the jacket.
  • a tube ll connected to a vacuum pump I? whereby a pressure of about 20 ms. of mercury is maintained within the apparatus.
  • the total energy radiated from the cover I2 is proportional to the fourth power of its absolute temperature, an increase in the temperature of the cover results immediately in a more intense radiation. As a result the temperature of the cover can be maintained substantially constant. This is of thegreatest importance for the condensation of the sublimate so that the actual temperature of the cover may fluctuate only between narrow limits.
  • the temperature of the cover is a function of the intensity of the radiation and this intensity can be increased or decreased by means which are known per se.
  • the outer surface of the cover may be provided with a coat of dead-black paint i6, or cooling ribs and the like may be provided.
  • the temperature of the cover i2 is temporarily too low, for example is slow in reaching the desired value at the beginning of the process, it can be rapidly increased to the desired value by causing part of the high-frequency field to extend through a portion of the cover.
  • the winding 8 may be placed higher so as to surround the lower part of cover i2.
  • I have found that this is generally unnecessary, because the heat developed by the condensation of the sublimate is usually sumcient. Therefore, I generally locate the cover outside the high-frequency field, as shown.
  • a vacuum sublimating apparatus comprising a crucible of non-metallic material adapted to receive the material to be Sublimated, means to produce high-frequency current for heating the material to be Sublimated, a dome-shaped metal cover on said crucible and serving as a condensing member for the vapors of the sublimate, said cover being tightly jointed to the crucible and being provided with an outlet opening, the spaces within the cover and crucible being connected by a passageway having a cross-sectional area approximately the same as the area of the free surface of the charge within the crucible, and means to remove heat from said cover substantially only by radiation, said means comprising a heat-receiving member surrounding said cover with an intermediate space, and a device for producing a low pressure within said space.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)
US298330A 1938-10-17 1939-10-06 Sublimating apparatus Expired - Lifetime US2252052A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB30057/38A GB520434A (en) 1938-10-17 1938-10-17 Improved method of and apparatus for sublimating materials at a low pressure

Publications (1)

Publication Number Publication Date
US2252052A true US2252052A (en) 1941-08-12

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ID=10301554

Family Applications (1)

Application Number Title Priority Date Filing Date
US298330A Expired - Lifetime US2252052A (en) 1938-10-17 1939-10-06 Sublimating apparatus

Country Status (5)

Country Link
US (1) US2252052A (enrdf_load_stackoverflow)
DE (1) DE717437C (enrdf_load_stackoverflow)
FR (1) FR862427A (enrdf_load_stackoverflow)
GB (1) GB520434A (enrdf_load_stackoverflow)
NL (1) NL54601C (enrdf_load_stackoverflow)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2429668A (en) * 1942-08-07 1947-10-28 Acme Aluminum Alloys Inc Metallurgical furnace and condenser
US2482127A (en) * 1946-08-07 1949-09-20 Us Interior Apparatus for refining metals
US2636915A (en) * 1952-04-07 1953-04-28 Nu Dent Porcelain Studios Inc Apparatus for vacuum firing of porcelain dental articles
US2745891A (en) * 1954-03-15 1956-05-15 Rem Cru Titanium Inc Apparatus for melting highly reactive metals
US2826624A (en) * 1956-12-05 1958-03-11 Stanton L Reese Vapor shield for induction furnace
US3132198A (en) * 1962-01-15 1964-05-05 Stauffer Chemical Co Electron beam furnace
US4264778A (en) * 1979-06-25 1981-04-28 Societa Italiana Per Il Magnesio E Leghe De Magnesio S.P.A. Extraction furnace

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1021978B (de) * 1953-04-08 1958-01-02 Philips Nv Verfahren zur Reindarstellung bzw. Trocknung von biologischen Praeparaten durch Trennen einer fluechtigen Substanz aus Substanzgemischen
US3202485A (en) * 1962-05-01 1965-08-24 Alton F Armington Sublimation apparatus

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2429668A (en) * 1942-08-07 1947-10-28 Acme Aluminum Alloys Inc Metallurgical furnace and condenser
US2482127A (en) * 1946-08-07 1949-09-20 Us Interior Apparatus for refining metals
US2636915A (en) * 1952-04-07 1953-04-28 Nu Dent Porcelain Studios Inc Apparatus for vacuum firing of porcelain dental articles
US2745891A (en) * 1954-03-15 1956-05-15 Rem Cru Titanium Inc Apparatus for melting highly reactive metals
US2826624A (en) * 1956-12-05 1958-03-11 Stanton L Reese Vapor shield for induction furnace
US3132198A (en) * 1962-01-15 1964-05-05 Stauffer Chemical Co Electron beam furnace
US4264778A (en) * 1979-06-25 1981-04-28 Societa Italiana Per Il Magnesio E Leghe De Magnesio S.P.A. Extraction furnace

Also Published As

Publication number Publication date
NL54601C (enrdf_load_stackoverflow) 1943-05-15
FR862427A (fr) 1941-03-06
GB520434A (en) 1940-04-24
DE717437C (de) 1942-02-13

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