US2892759A - Distillation flask and mounting - Google Patents

Distillation flask and mounting Download PDF

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US2892759A
US2892759A US647662A US64766257A US2892759A US 2892759 A US2892759 A US 2892759A US 647662 A US647662 A US 647662A US 64766257 A US64766257 A US 64766257A US 2892759 A US2892759 A US 2892759A
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flask
housing
heater
distillation
rods
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US647662A
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Nerheim Arvie Glenn
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Standard Oil Co
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Standard Oil Co
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/14Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S159/00Concentrating evaporators
    • Y10S159/07Magnetic coupling

Description

3 Sheets-Sheet l June 30, 1959 A. G. NERHEIM I DISTILLATION FLASK AND MOUNTING Filedmamh 21,Y 1957 9%' fwd@ June 30, 1959 A. G. NERHEIM 2,892,759

DISTILLATIGN FLASK AND MOUNTING Filed March 2i, 1957 s sheets-sheet 2 June 30, 1959 A. G. NERHEIM 2,892,759

` DISTILLATION FLASK AND MOUNTING Filed March 21, 1957V v5 Sheets-Sheet 5 lama Mmeg

DISTILLATION FLASK AND MOUNTING Arvie Glenn'Nerhem, Calumet City, Ill., assignor to Standard Oil Company, Chicago, Ill., a corporation of Indiana Application March 21, 1957, Serial No. 647,662

3 Claims. (Cl. 202-235) This invention relates to improved fractionator columns of the type known as lspinning band columns. More particularly, the invention relates to distilling flask constructions for such a fractionator.

In a spinning band column, the complete unit comprises in general a still pot for holding the charge, a fractionating column or tube, a condenser system, a liquid product receiver, and a rotatable element disposed within the fractionating column. Conventionally, spinning band columns of the type to which my improvements relate employ a rotatable element comprising a metallic band having a cross-sectional area which is substantially less than the flow area of the column. Controllable heating means are provided for supplying heat to the still pot, the still pot and heating element ordinarily being enclosed withina vacuum liask which is removably seated at its upper end in contact with a vacuum jacket which substantially encloses the fractionatng column and take-off line. Throughput in a spinning band column is conventionally controlled by controlling the heaters; however, it has been found that column eiiiciency may be increased by increasing the rotation speed of the spinning band. However, if vibration occurs in spinning band columns and if frictional heat of Yrotation is generated, the eiiiciency is lower.

4Distilling flask assemblies heretofore used are not easily recharged and further misalignment of the distilling flask assembly may break the column-flask joint. Bumping the flask out of alignment or attempting to remove a flask frozen to the column also have resulted in breaking the column-flask joint.

' It is therefore, an object of my invention to provide a distilling flask assembly which avoids these difliculties. Thus, it is a further object of the invention to provide a distilling flask assembly which will permit recharging of the sample, which gives protection to the column, which is less expensive and ofsimpler construction than heretofore used, and which may be adapted for use on conventional fractionating columns. The above and other objects of the invention will become apparent as the detailed description thereof proceeds. Y

Further details and advantages of my invention will become apparent as the description thereof proceeds with reference to the accompanying drawings wherein:

Figure 1 is a vertical section showing the spinning band drive, head construction and distillation iiask;

Figure 2 is a top view, partly in section, of the head viewed along the line 2 2 with parts removed in Figure 1;

Figure 3 is an elevation, partly in section, of the adjustable ask support;

Figure 4 is a side view of the apparatus in Figure 3;

Figure 5 is a section taken along line 5--5 in Figure 3;

Figure 6 is a fragmentary side elevation taken along the line 6-6 in Figure 3; and

Figure 7 is a fragmentary plan view, taken along the line 7-7 in Figure 3.

Referring to Figures l and 2 of the drawings, a column ate t 10 comprising a relatively long thin glass tube, contains the spinning band llhaving a drive shaft 12 which extends through the head 13 and is secured to the drive pin 14 within the magnetic coupling 15. This coupling 15 includes a pair of opposed magnets 16 and 17 arranged axially of each other and of the shaft 12. The drive magnet 16 is secured, for example, by a chuck means 13 so that it may be driven, and the other magnet 17 is within a vacuum-tight and non-magnetic housing 19 which is fixed to the head 13 by means of a standard tapered joint 20 engaging a corresponding tapered joint 21 in head 13.

The elongated drive pin 14 disposed within the separable housing 19 is arranged to be rotated with the enclosed magnet 17. An antifriction bearing means 22 rotatably supports the drive pin 14 within the housing 19. The drive shaft 12, xed to drive pin 14, extends longitudinally from the lower end of the housing 19, through the head 13, and engages tfhe band shaft 23 which in turn supports the rotatable element on band 11.

The rotatable band 11 is slightly smaller in its greatest lateral dimension than the internal diameter of the fractionating tube or column 10. Rotation of the close-itting band 11 produces a wetted wall effect within the fractionating tube 10 with the result that there is intimate contact between the up-flowing vapors within the column 10 and the down-ilowing reflux on the wall thereof.

The head 13 includes a tapered body 24 arranged in a vacuum-tight seal with the seat 2S at the upper end of the column 10. The head 13 includes laterally-extending condenser inlet 26 and outlet 27, each passing through the side wall thereof and being connected to opposite ends of the looped condenser 28 which depends below the hollow body 24 into the top of the column 10. A drip tip 29 is provided on each of the separate legs of the condenser 28. A vacuum connection 30, also laterally extending from the side wall of head 13, permits vacuum operation of the column 10' and completes the construction of head 13.

The leads 31 to thermocouple 32 pass through the housing 19 and the therrnocouple 32 is disposed adjacent the upper end of the spinning band 11 and soldered in place. The solenoid 33 is aligned with the soft iron core 34 embedded within a cavity 35 in housing 19. Immediately below the exposed inner end of the core 34 is arranged the upper paramagnetic end 36 of the needle shaft 37 which passes within the needle guide bore 39 in housing 19 and the needle tip 40 is on the needle seat 41. The needle tip 40 is thus raised from the seat 41 by the action of the electromagnet bar or core 34 on the paramagnetic top 36 of the needle 37 when the solenoid coil 33 -is energized.

A condenserv 28 comprises a loop of tubing which doubles back on itself with a pair of drip tips 29 at the lower extremities of the loop which discharges on the edge of the needle seat 41. When the needle tip 40 is raised from the seat 41, the condensate is removed from the column by take-oid:` line 42 into a receiver (not shown). By regulating the ow of cooling fluid into the total condenser 28, the evolved vapors within the fractionating tube 10 may be condensed and returned as reiiux when the take-olf line 42 is closed by the needle valve.

Condensate is prevented from leaking past the needle seat 41 by alignment of the needle 37 and by keeping the tip 46 clean. The head 13 should be adjusted rso that the needle 37 is vertical and moves freely within the guide bore 39. It will be understood that the paramagnetic end 36 of the needle 37 is disposed immediately below the inner end of the bar 34 and is lifted thereby when the coil 33 is energized.

Referring to Figures 3 to 7 showing the distillation flask and mounting, I provide a flask 50 which is simply set on a heater 51. An insulating dewar flask 52 contains the distilling fiask 50, and a glass wool collar 53 closes the flask 52. The distillation flask 50 is provided with a thermocouple well 54 and the thermocouple leads 55 extend over the top of the dewar ask 52. The heater 51 is supported by a coil spring 56 disposed within the dewar flask 52. The heater leads 57 pass through the glass wool collar 53 and from the dewar flask 52.

The flask 50 is pear-shaped and set in a cone-shaped heater 51 mounted on a spring 56. The entire apparatus is insulated with a dewar ask S2 and a glass wool collar 53. A support device 58 yfor the flask 52 is secured to the dewar flask 52 permitting it to be swung directly under the column and up into the aligning guide 59 which positions the flask for charging. The contents of the ask l5i) are stirred with a wire impellor V68 fixed to the .lower end of the spinning band 11.

The aligned distilling ilask 50 is fixed to the lower end of the column 10. The dewar flask 52 is lifted by raising the mounting 58 on the 'slide rods 61 and .disposed about the distilling flask 50 thereby providing effective insulation throughout the distillation.

The particular elements of the apparatus covered by Figures 3 to 8 are the slide rods 61 with aligning guide 59, flask 'support device 58, the heater 51 and flask 50. The tops of the two slide rods 61 are secured with connectors 68 welded to the edges of a clamp 69 which is bolted to the column support 70 just above the ask joint 71. The bottom of slide rods 61 are set in the foot 72 welded to a base 73 below the column 10. The aligning guide 59, comprising a metal strip welded to a connector 68, is fastened to the right slide rod 61.

The flask support device 58 pivots around the left slide rod 61 on a leveling apparatus 74 (Figures 3 and 5) that pinches the rod 61 to hold the support 58 ata desired height above the base 73. The support 58 clamps around a pint dewar flask 52 with support lip 76 sliding up under the aligning guide 59 to steer the support 58 as it is raised to the desired position below the column 10.

The heater 51 is a metal cone Wound with high resistance wire and insulated. Two clamps 77 protect this wiring and hold the supporting coil spring 56 in place. .A variety of flask sizes ranging from 25-200 ml. may be used. If the ask freezes to the column, it can be removed easily by simply heating the ask .joint with a torch.

When the distillation is complete, the dewar ask 52 can be lowered on support 58 and this quickly cools the distilling flask 50 which permits its prompt removal from the column .10. These features permit more eflicient distillation in less time and at less cost than distillation ilask assemblies heretofore used with spinning band columns.

The appartus has been described as including an eX- terior permanent magnet. An electromagnet may be substituted on the housing, enclosing the interior permanent magnet, surrounded by field windings so that the enclosed magnet comprises a rotor or amature of a motor.

This application is a continuation-impart of my now abandoned application Serial No. 596,584, filed July 9, 1956, and entitled Spinning Band Fractionator.

Although the invention has been described with reference to a preferred embodiment thereof, it is to be understood that this is by way of illustration only. Accordingly, it is contemplated that modifications and variations can be made in the apparatus by those skilled Ain the artin light of the preceding description and without departing from the spirit ofthe invention.

What I claim is:

1. An improved distillation flask assembly which comprises in combination a pear-shaped distillation flask, a standard tapered joint in the upper end of said distillation flask, a well in the lower end of said flask, a cone heater for said ask disposed about the lower end thereof and encircling said well, an open-topped insulating housing accommodating said heater and said flask, coil spring support means between the bottom end of said housing and said heater, a removable insulating collar enclosing the top of said housing and encircling the upper end of said flask, an adjustable support for said housing, said adjustable support including a base, a pair of upstanding rods on said base, a swingable clamping arm hingedly xed to one of said rods, vertical guide means carried by the second of said rods, a projection of said clamping arm adapted to move within said guide, said guide means comprising an open-ended slot terminating above said base and open at its lower end to pass said projection, and means associated with said Vhingedly fixed arm for vertically adjusting said support.

2. An improved distillation flask support assembly including a base, a pair of spaced upstanding rods on said base, a horizontally swingable clamping arm hingedly fixed to one of said rods, vertical guide means carried by the second of said rods and terminating a substantial distance above said base, a projection in said clamping arm adapted to move vertically within and below `said guide means, and means associated with said hingedly fixed clamping arm for vertically adjusting said support assembly downwardly below said guide means to permit horizontal rotation of said arm.

3. A distillation flask assembly and retractable -support Vtherefor which comprises a distillation ask having a constricted bottom portion, a cone heater for said flask disposed about and below said bottom portion, an insulated housing containing said heater and said flask, a retractable support for said housing, said support including a horizontal swingable clamping arm, arrst upright slide rod, vertically adjustable friction holder means securing Asaid arm to said slide rod, a second slide rod parallel to said first slide rod, an aligning guide member supported by said second slide rod, said guide member being substantially shorter than said slide rod and secured thereto only at its upper end, a guide tongue carried by the outer end of said arm, Vsaid tongue and said aligning guide member cooperating to normally restrain said arm against horizontal rotation, whereby lowering said arm by adjustment of said friction holder means retractssaid tongue from within said guide member thereby permitting the horizontal nrotation of said arm and said insulated housing containing lsaid ask and heater.

Laboratory for the Synthetic Liquid Fuels Program, (Feldman, Pantazoplos, and Orchin), Bureau of Mines, Report of Investigations 4764 (Fig. 2 relied on).

Claims (1)

1. AN IMPROVED DISTILLATION FLASK ASSEMBLY WHICH COMPRISES IN COMBINATION A PEAR-SHAPED DISTILLATION FLASK, A STANDARD TAPERED JOINT IN THE UPPER END OF SAID DISTILLATION, A WELL IN THE LOWER END OF SAID FLASK, A CONE HEATER FOR SAID FLASK DISPOSED ABOUT THE LOWER END THEREOF AND ENCIRCLING SAID WELL, AN OPEN-TOPPED INSULATING HOUSING ACCOMMODATING SAID HEATER AND SAID FLASK, COIL SPRING SUPPORT MEANS BETWEEN THE BOTTOM END OF SAID HOUSING AND SAID HEATER, REMOVABLE INSULATING COLLAR ENCLOSING THE TOP OF SAID HOUSING AND ENCIRCLING THE UPPER END OF SAID FLASK, AN ADJUSTABLE SUPPORT FOR SAID HOUSING, SAID ADJUSTABLE SUPPORT INCLUDING A BASE A PAIR OF UPSTANDING RODS ON SAID BASE, A SWINGABLE CLAMPING ARM HILNGEDLY FIXED TO ONE SAID RODS, VERTICAL GUIDE MEANS CARRIED BY THE SECOND OF SAID RODS, A PROJECTION OF SAID CLAMPING ARM ADAPTED TO MOVE WITHIN SAID GUIDE, SAID GUIDE MEANS COMPRISING AN OPEN-ENDED SLOT TERMINATING ABOVE SAID BASE AND OPEN AT ITS LOWER END TO PASS SAID PROJECTION, AND MENS ASSOCIATED WITH SAID HINGEDLY FIXED ARM FOR VERTICALLY ADUSTING SAID SUPPORT.
US647662A 1957-03-21 1957-03-21 Distillation flask and mounting Expired - Lifetime US2892759A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080173531A1 (en) * 2006-06-16 2008-07-24 Kesler Michael L Distillation apparatus and method of use

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2190220A (en) * 1939-06-12 1940-02-13 Ace Glass Inc Chemical apparatus
US2573807A (en) * 1946-11-08 1951-11-06 Sinclair Res Lab Inc Still
US2608528A (en) * 1949-03-11 1952-08-26 Sinclair Res Lab Inc Microstill
US2764534A (en) * 1955-05-11 1956-09-25 Standard Oil Co Head for spinning band fractionator
US2783401A (en) * 1952-09-11 1957-02-26 Standard Oil Co Seal and magnetic drive

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2190220A (en) * 1939-06-12 1940-02-13 Ace Glass Inc Chemical apparatus
US2573807A (en) * 1946-11-08 1951-11-06 Sinclair Res Lab Inc Still
US2608528A (en) * 1949-03-11 1952-08-26 Sinclair Res Lab Inc Microstill
US2783401A (en) * 1952-09-11 1957-02-26 Standard Oil Co Seal and magnetic drive
US2764534A (en) * 1955-05-11 1956-09-25 Standard Oil Co Head for spinning band fractionator

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080173531A1 (en) * 2006-06-16 2008-07-24 Kesler Michael L Distillation apparatus and method of use
US7976699B2 (en) 2006-06-16 2011-07-12 Kesler Michael L Distillation apparatus and method of use

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