US2137553A - Apparatus for high-vacuum distillation - Google Patents

Apparatus for high-vacuum distillation Download PDF

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Publication number
US2137553A
US2137553A US85410A US8541036A US2137553A US 2137553 A US2137553 A US 2137553A US 85410 A US85410 A US 85410A US 8541036 A US8541036 A US 8541036A US 2137553 A US2137553 A US 2137553A
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United States
Prior art keywords
plates
members
evaporating
troughs
pumps
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 - Lifetime
Application number
US85410A
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English (en)
Inventor
Vigers Brian Edmund Allen
Mccowen John Lewis
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Imperial Chemical Industries Ltd
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Imperial Chemical Industries Ltd
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Publication date
Application filed by Imperial Chemical Industries Ltd filed Critical Imperial Chemical Industries Ltd
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Publication of US2137553A publication Critical patent/US2137553A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/12—Molecular distillation

Definitions

  • the invention relates to an improved apparatus for carrying out short-path high-vacuum distillation.
  • the general conditions for carrying out distillations of this type are, firstly that the distillation is effected .under an extremely high vacuum of the order of 10- to 10 mms. of mercury, and secondly that the evaporating and condensing surfaces inside the still are in close proximity, usually about 1 to 5 cms. apart. It is known to construct the evaporating and condensing surfaces as vertical surfaces, down which flow respectively the liquid to be distilled and the condensate, either by employing a concentric tube arrangement or by employing flat-surfaced plates or blocks.
  • the present invention provides a. construction of apparatus which meets these desiderata, and is, in general, an improvement over existing types of still.
  • an apparatus for effecting short-path high-vacuum distillation comprises a number of parallel plates or blocks, the faces of which provide the evaporating and condensing surfaces, the said plates or blocks being supported in a vertical or inclined position, from a headstock, that is a combined support and closure member, through which substantially all pipe and other connections necessary for the working of the still are made, while the assembly of plates or blocks together with their attendant feeding and collecting apparatus is enclosed by a vacuum-tight casing, preferably a cylindrical casing, making a single vacuum-tight joint at the headstock.
  • the plates or blocks are suitably formed with tubular or hollow passages in order to permit of the passage of heating or cooling media. Where the headstock is arranged vertically and the casing is horizontal, it may be mounted on wheels running on rails, so that it may be easily retracted for inspection.
  • Figures 1 and 2 are diagram: matic sectional side and end elevations respectively of the apparatus.
  • the evaporating plates l and the condensing plates 2 are carried in the desired positions by the cantilever truss 3, which is attached tq the headstock frame 4.
  • the whole assembly of plates is enclosed by a cylindrical casing 5, which makes a vacuum-tight joint at 6 with the headstock.
  • the headstock thus serves as a closure for the casing as well as a support for the plates;
  • the arrangement of rectangular plates in a casing of circular cross-section provides four segmental spaces around the plate'assembly.
  • troughs I, 8 and 9. The material to be distilled is fed into the main trough I by the pipe I 0 passing through the headstock 4, and is thence distributed by the .troughs 8 and 9 to the tops of the evaporating plates I.
  • Troughs are provided integral with or attachedto the tops of the evaporating plates and the feed to the latter is by a series of weir notches 3
  • the condensing plates rather larger than the evaporating plates, the top edges of the former having ridges as indicated at 32 arranged to act as bafiles to catch molecules escaping from the ends of the evaporating plates, and from the gap between the plates, into the evacuated space. which would not otherwise strike the cooling surfaces.
  • This arrangement of the condensing plates also facilitates the attaining of the necessary high vacuum.
  • the first stage or stages of evacuation pumps l5 may be arranged.
  • Such pumps may be of the molecular diffusion or condensation type, supplemented by a backing pump, the
  • backing connections l6 being carried out through the headstock and connected to an appropriate backing pump (not shown), for the purpose of producing as high a vacuum as possible within the apparatus.
  • Cooled baflies Il may be provided over the intakes of the pumps l 5.
  • Hot oil for heating the evaporating plates is introduced by the pipe l8 and removed by the pipe I?
  • the plates are shown as having tubular 2 passages 32 for conducting the hot oil (Figs. 1 and 2).
  • Cold water for cooling the condensing plates is introduced by the pipe 20 and removed,
  • the condensing plates are similarly formed with tubular passages, 34, for the cooling water.
  • come out througlr the headstock, although not shown in Figure 1.
  • the heating and cooling media are conducted to their appropriate plates by pipes 22, which are preferably of considerable length in order that their elasticity may permit of slight movements due to temperature changes.
  • joints 23, preferably of the metallic lens ring type, may be introduced in the pipes 22.
  • distillation apparatus can be applied for the purpose of a multi-stage still, in which case the necessary pumping arrangements are provided for trans ferring distillate or residue or both from one stage to another, such pumps being located in the bottom segmental space at 24.
  • These pumps may be driven by electrical means; or by means of a common driving shaft brought out through the headstock by a gland and connected to a suitable source of power.
  • Apparatus for carrying out short-path high vacuum distillation comprising a plurality V of plate-like members in parallel arrangement and having opposed substantially vertical parallel faces, means for heating alternate members so as to provide evaporating surfaces, means for cooling the members intermediate the heated members so as to provide condensing surfaces opposed to said evaporating surfaces, a casing and. a closuremember making a' vacuum-tight joint with the casing, the casing and closure member defin- .duit means extending through the closure member into the chamber forfeeding raw 'material to the upper portion of the heated members, and
  • Apparatus for carrying out short-path high vacuum distillation comprising a plurality of rectangular plate-like members having opposed, parallel faces arranged for flow of liquids downward thereover by gravity, means for heating alternate members to provide evaporating surfaces, means for cooling intermediate members to provide condensing surfaces, a housing for said members, troughs provided above the evaporating members and arranged to deliver liquid to be distilled over the surfaces of the evaporating members, a closure member for the housing arranged to support said plate-like members, the closure member and housing defining a vacuumtight chamber surrounding the plate-members, collecting troughs below the ,members arranged to collect separately the liquid condensate and orating members respectively, and conduit means communicating with said troughs and passing through the closure member for separately withdrawing condensate and residue.
  • condensing members are provided with ridges at their top extending beyond the tops of the evaporating members and serving as baffles to catch molecules escaping from the ends of the evaporating members and from the gap between the members.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
US85410A 1935-06-14 1936-06-15 Apparatus for high-vacuum distillation Expired - Lifetime US2137553A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB17173/35A GB458117A (en) 1935-06-14 1935-06-14 Improvements in and relating to apparatus for high vacuum distillation

Publications (1)

Publication Number Publication Date
US2137553A true US2137553A (en) 1938-11-22

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ID=10090546

Family Applications (1)

Application Number Title Priority Date Filing Date
US85410A Expired - Lifetime US2137553A (en) 1935-06-14 1936-06-15 Apparatus for high-vacuum distillation

Country Status (5)

Country Link
US (1) US2137553A (enrdf_load_html_response)
BE (1) BE418818A (enrdf_load_html_response)
FR (1) FR815150A (enrdf_load_html_response)
GB (1) GB458117A (enrdf_load_html_response)
NL (1) NL44902C (enrdf_load_html_response)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2587260A (en) * 1948-05-27 1952-02-26 Phillips Petroleum Co Apparatus for molecular distillation
US2703310A (en) * 1953-12-03 1955-03-01 Givaudan Corp Apparatus for molecular distillation
DE3122652A1 (de) * 1981-06-06 1982-12-23 Leybold-Heraeus GmbH, 5000 Köln Verfahren und vorrichtung zur kurzweg-destillation
DE3122651A1 (de) * 1981-06-06 1982-12-23 Leybold-Heraeus GmbH, 5000 Köln Vorrichtung zur kurzweg-destillation
US4504361A (en) * 1981-06-22 1985-03-12 Slovenska Vysoka Skola Technicka V Bratislava Block short-way evaporator with wiped-off film

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2587260A (en) * 1948-05-27 1952-02-26 Phillips Petroleum Co Apparatus for molecular distillation
US2703310A (en) * 1953-12-03 1955-03-01 Givaudan Corp Apparatus for molecular distillation
DE3122652A1 (de) * 1981-06-06 1982-12-23 Leybold-Heraeus GmbH, 5000 Köln Verfahren und vorrichtung zur kurzweg-destillation
DE3122651A1 (de) * 1981-06-06 1982-12-23 Leybold-Heraeus GmbH, 5000 Köln Vorrichtung zur kurzweg-destillation
US4504361A (en) * 1981-06-22 1985-03-12 Slovenska Vysoka Skola Technicka V Bratislava Block short-way evaporator with wiped-off film

Also Published As

Publication number Publication date
GB458117A (en) 1936-12-14
BE418818A (enrdf_load_html_response)
NL44902C (enrdf_load_html_response)
FR815150A (fr) 1937-07-06

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