US1693243A - Method and apparatus for purifying camphor and similar volatile substances - Google Patents

Method and apparatus for purifying camphor and similar volatile substances Download PDF

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US1693243A
US1693243A US52953A US5295325A US1693243A US 1693243 A US1693243 A US 1693243A US 52953 A US52953 A US 52953A US 5295325 A US5295325 A US 5295325A US 1693243 A US1693243 A US 1693243A
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camphor
chamber
gas
purifying
volatile substances
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Evarts G Loomis
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/783Separation; Purification; Stabilisation; Use of additives by gas-liquid treatment, e.g. by gas-liquid absorption

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  • the object of my invention is to ⁇ provide a' method of treating camphor and similar readily v'oatilized materials so as to remove undesirable impurities and also to. provide an apparatus which isasiii'tble for carrying out this method. This object is accomplished by my invention, one embodiment of which is hereinafter more particularly set forth.
  • My improved apparatus 1 in the embodiment shown, is provided with a preliminary heating vessel 2,a retort 3, a. condensing chamber 4, a gas heater 5, a blower 6 and suitable valves and pipes, as will appear below.
  • the camphor or other material, the term camphor being used throughout to indicate any material suitable for the'apparatus, is first loaded in the preliminary heating vessel 2 by removing the cover 31. .It is then heated so as to drive off all water vapor T and low temperature volatile impurities which can escape through a. valve 7 at the top which may be opened by hand for this purpose. Heavy and nonfusible impurities are also separated in this preliminary heating vessel by their being allowed to settle to the bottom,
  • the vessel 2 is preferably provided with a steam jacket 9, or other heating means, with steam entering at 10 and escaping at 11, in the conventional a5 manner.
  • a valve 12 in youtlet pipe 13 may then be opened so as to ermit drainage from the vessel 2 through t e pipe 13 which may also be steam jacketed so as to prevent its becoming clogged 46 with solidified material.
  • This pipe 13 runs to the retort 3 which is heated by means of a steam jacket 14 which receives steam at 15 and allows it to escape at 16, in the conventional manner.
  • the camphor 18, which has first been heated in the vessel 2 is, as above described, drained into the retort 3 to substantially the extent indicated, that is below the air or gas inlet pipe 19.
  • This pipe has downwardly disposed openings through which air or an inert gas, such as nitrogen or carbon lioxide,is admitted under slight pressure;
  • an inert gas such as nitrogen or carbon lioxide
  • the purpose of substituting an inert gas instead of Iair is to avoid the danger of forming explosive mix-l "0 tures.
  • air is used with the understanding that for the purposes of this case such an linert gas is e uivalent.
  • the air from the pipe 19 enters under pressure and in impinging against the hot surface of the liquid camphor 18, it comes in intimate contact withandmore or less saturated with the camphor in the form of vapor which it lm out of the vessel through an exhaust ipe 20v which contains a valve 21 by which the assage through this pipe maybe contro ed.
  • This pipe 20 runs tot e condensing chamber 4 which is a large chamber with metal walls and a large-radiating surface on the exrterior of the metal so that the heat of the air with the camphor vapor is rapidly vdissipated so that the camphor will fallin flakes somef thing like snow upon the bottom of the chammn ber 4, leaving the air free-to pass out of the chamber through a chimney or Hue 22 to the heatin chamber 5 whichhas its exterior carefully insulated, as indicated at 23, and its interior provided with a heating pipe 24 with -105 a steam inlet 25 and outlet 26 so that the air assing aboutthis heating coil regainsthe heat lost in the condensing chamber 4 and thereupon this heated air passes through a lagged Dine 27 to the blower 6 which puts this lm air under pressure Vand Vforces the same into the lagged pipe 28 and through a valve 29 to the ipe 19 in theretort 3.
  • the actionl of this process depends on a iow of the air or gas which' acts as avehicle to carry .the pure camphor lfrom the retort 3 to thecondensingchamber,4. It will be noted f that the camphor is vaporized without the 'necessity of boiling and without'any agitation of any consequence so that impurities will not be released through violent boiling, or in any slmilar manner. l
  • means for heatin Lcamphor to a liquid state a chamber into W ich said heated camphor is passed, means'for passing gas u on the surface of the camphorfin said c amber and means for evacuating the mixture and caus-Y ing the same to cool.
  • a heating chamber having a steam jacket for melting camphor or similar material, a second chamber into which said heated-camphor is passed, means for passing'- a currentof gas upon, this melted material in said second chamber, means for receiving and cooling' this mixture, means for heating said gas and means for passin Ysaidheated gas back into said second cham r of melted camphor.
  • a preliminary eating chamber adapted to receive camphor or similar material and means for heating said lchamber so as to drive oif volatile impurities, means for permitting the escape of such impurities, a second :heatin chamber and means ⁇ for passing melte w camphoror similar material from the first to the second chamber, means for heating said Y,

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Description

E. G. LOOMIS METHOD AND APPARATUS FOR PURIFYING CAMPHOR AND SIMILAR VOLATILE SUBSTANCES Filed Aug. 27, 1925 ,mum o Nov. 27, 1928.
m d u n# MH N i QH Patented Nev. 27, 192s.
UNITED STATES y1,693,243l PATENT OFFICE.
EVABTS G. LOOIIS, 0F NEWARK, NEW JERSEY.
lMETHOD AND APPARATUS FOR PUBIFYING CAMPHOB AND SIMILAR VOLATILE SUBSTANCES. i
Application iiled August 27, 1925. Serial No. 52,953.
The object of my invention is to` provide a' method of treating camphor and similar readily v'oatilized materials so as to remove undesirable impurities and also to. provide an apparatus which isasiii'tble for carrying out this method. This object is accomplished by my invention, one embodiment of which is hereinafter more particularly set forth.
For a more particular description of my l0 invention, reference is to he had to the accompanying drawing, forming a part hereof, in which the gure shows an apparatus suitable for carrying out my improved method.
My improved apparatus 1, in the embodiment shown, is provided with a preliminary heating vessel 2,a retort 3, a. condensing chamber 4, a gas heater 5, a blower 6 and suitable valves and pipes, as will appear below. Briefly stated, the camphor, or other material, the term camphor being used throughout to indicate any material suitable for the'apparatus, is first loaded in the preliminary heating vessel 2 by removing the cover 31. .It is then heated so as to drive off all water vapor T and low temperature volatile impurities which can escape through a. valve 7 at the top which may be opened by hand for this purpose. Heavy and nonfusible impurities are also separated in this preliminary heating vessel by their being allowed to settle to the bottom,
below the outlet pipe 13. f The vessel 2 is preferably provided with a steam jacket 9, or other heating means, with steam entering at 10 and escaping at 11, in the conventional a5 manner. After vthe camphor has been inserted through the cover 31, and this cover has been closed and heat '.-has been, applied so as to vaporize such impure volatile products which have been al owed to escape, as
above set forth, and the camphor liquefied, a valve 12 in youtlet pipe 13may then be opened so as to ermit drainage from the vessel 2 through t e pipe 13 which may also be steam jacketed so as to prevent its becoming clogged 46 with solidified material. This pipe 13. runs to the retort 3 which is heated by means of a steam jacket 14 which receives steam at 15 and allows it to escape at 16, in the conventional manner.
5o hand hole 17 which corresponds .to a hand hole 8 in the heating vessel 2 and is closed in 4the same manner. It permits ready access for the purpose of cleaning and removing residual impurities from time to' time, as
65 may be necessary. After theretort 3 has recarries away in a very pure form as it passes The retort 3 is provided with aceived its charge valve 12 is closed and a new lotof crude camphor may be loaded into chamber 2 which in turn may betreated as the first in preparation for the retort when it is ready for its second charge.
The camphor 18, which has first been heated in the vessel 2 is, as above described, drained into the retort 3 to substantially the extent indicated, that is below the air or gas inlet pipe 19. This pipe has downwardly disposed openings through which air or an inert gas, such as nitrogen or carbon lioxide,is admitted under slight pressure; The purpose of substituting an inert gas instead of Iair is to avoid the danger of forming explosive mix-l "0 tures. l A The term air is used with the understanding that for the purposes of this case such an linert gas is e uivalent. This air is allowed to If the camphor hea-ted to a higher temperature and made to boil, bubbles would be given ofi', which in bursting would throw up dirt and impurities in the current of air, which im- B0' purities would be liable to escape from the f retort 3. It is intended that these impurities" should remain in the retort 3 and be removed from time to-timethrough the hand hole-17. The air from the pipe 19 enters under pressure and in impinging against the hot surface of the liquid camphor 18, it comes in intimate contact withandmore or less saturated with the camphor in the form of vapor which it lm out of the vessel through an exhaust ipe 20v which contains a valve 21 by which the assage through this pipe maybe contro ed. This pipe 20 runs tot e condensing chamber 4 which is a large chamber with metal walls and a large-radiating surface on the exrterior of the metal so that the heat of the air with the camphor vapor is rapidly vdissipated so that the camphor will fallin flakes somef thing like snow upon the bottom of the chammn ber 4, leaving the air free-to pass out of the chamber through a chimney or Hue 22 to the heatin chamber 5 whichhas its exterior carefully insulated, as indicated at 23, and its interior provided with a heating pipe 24 with -105 a steam inlet 25 and outlet 26 so that the air assing aboutthis heating coil regainsthe heat lost in the condensing chamber 4 and thereupon this heated air passes through a lagged Dine 27 to the blower 6 which puts this lm air under pressure Vand Vforces the same into the lagged pipe 28 and through a valve 29 to the ipe 19 in theretort 3. y
' e action of this apparatus, as above described, is carried on until all the campho in the retort 3 has been evaporated, when the blower 6 is stopped and a new charge of melted camphor is introduced from heating chamber 2, as heretofore described and the operation repeated. When the impurities in the heating vessel 2 or retort 3 require removal, this may be done through the manholes 8 and 17, respectively. Also the door of the condensing chamber 4 may be o ened and the camphor removed whenever su cient has collected. This may be done most conveniently when' the retort has become empty when the blower 6 is stopped and the valves 12, 29 and 21 are closed. The above sequence of operations may be repeated indefinitely. The actionl of this process depends on a iow of the air or gas which' acts as avehicle to carry .the pure camphor lfrom the retort 3 to thecondensingchamber,4. It will be noted f that the camphor is vaporized without the 'necessity of boiling and without'any agitation of any consequence so that impurities will not be released through violent boiling, or in any slmilar manner. l
ile I have shown and described one embodiment' of my invention, Iit is obvious that it is not restricted thereto, but that it is broad enough to cover all structures that come within the scope of the annexed'claiins.
Having thus described my invention, what Iclaimis: f'
1. The process of purifying camphor and similar substances which consists in reducing the camphor to a liquid form, forcing a current of gas below the boiling point of-V the camphor upon'the surface of the same and. thereb," causing the gas to become saturated with t e camphor vapor and then evacuating the mixture into a condensing chamber at a lower Vtemperature where the gas and 'camphor will 'separate and the -cam hor condense.
2. The process of purifymg camphor which consistsin heating a gas below the boiling point ofthe .c amphor and then assing the gas u on. the surface of melte where, y the camphor and gas will mix, an
' thereafter evacuating the mlxture'int a condensing chamber where the camphorfwill con-` 'conducting camphor e v my hand this thday of Yilugust'1925.
,gas and camphor vapor will mix and thereafter evacuating the-mixture to a condensing chamber. l l
4. In an apparatus of the class described, means for heatin Lcamphor to a liquid state, a chamber into W ich said heated camphor is passed, means'for passing gas u on the surface of the camphorfin said c amber and means for evacuating the mixture and caus-Y ing the same to cool.
5. In an apparatus of the class described, a heating chamber having a steam jacket for melting camphor or similar material,a second chamber into which said heated-camphor is passed, means for passing'- a currentof gas upon, this melted material in said second chamber, means for receiving and cooling' this mixture, means for heating said gas and means for passin Ysaidheated gas back into said second cham r of melted camphor.
6. In an 4ap aratusof the class described, v
a preliminary eating chamber adapted to receive camphor or similar material and means for heating said lchamber so as to drive oif volatile impurities, means for permitting the escape of such impurities, a second :heatin chamber and means `for passing melte w camphoror similar material from the first to the second chamber, means for heating said Y,
second chamber, means for passin a heated densing chamber connectedl to said evacuat` ing means, a'heatingchamber for receiving s, a yblower connected to sald heatmg cha-m r for drawing the as from said .chamberend a'pipe connecte to said blower for the 'heated gas 'to said second chamber.m"
In testimon i' whereof, I have hereunto .Evnnrs e. Ii-100.15413-Y
US52953A 1925-08-27 1925-08-27 Method and apparatus for purifying camphor and similar volatile substances Expired - Lifetime US1693243A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2608472A (en) * 1948-01-29 1952-08-26 Stokes Machine Co Sublimation apparatus

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2608472A (en) * 1948-01-29 1952-08-26 Stokes Machine Co Sublimation apparatus

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