Separatory Funnel

Abstract

Separatory funnel devices wherein either an upper liquid layer or a lower liquid layer can be selectively removed. These may be removed using the same or different conduits or stopcock valves. The devices consist essentially of an adjustable conduit which extends up into the flask portion of the separatory funnel for removing at least the upper liquid layer. For removing the lower liquid layer there may be a separate conduit and valve, or the same conduit extending up into the flask may be used. However, in any embodiment, either the upper liquid layer or lower liquid layer may be rapidly and easily removed.

Description

This invention relates to a type of liquid separating device, that is, a device for separating at least two liquids from each other. In particular, it relates to a separatory funnel device for separating at least two immiscible liquids of differing specific gravities one from the other.

There are various methods for separating two liquids present in two distinct layers. The most simple method is a decantation of one layer from the other. However, this is generally not a very accurate and effective method. There will not be an exact separation of one layer from another and such procedures are time consuming. Conventional laboratory type separatory funnels are an improvement on decantation methods in regard to the exactness of separation; but the use of such devices is tedious and is time consuming. Further, in these devices the lower layer must be removed first with partial contamination of the upper layer since it will intermix in the stem with residual amounts of the lower layer.

The prior patent art in regard to the devices of this invention is exemplified by U.S. Pats. No. 2,170,411, and No. 3,257,170. U.S. Pat. No. 2,170,411 discloses the use of segmented separatory flasks wherein differing levels can be removed. However, in this arrangement the takeoffs are at set heights so that if the liquid levels are intermediate to a drain opening, the removal will not be complete. U.S. Pat. No. 3,257,170 discloses a separatory funnel having an internal conduit; but this conduit is not adjustable and would not be effective for removing an upper liquid level. In general, those in the art appear to have accepted the shortcomings of separatory funnels and have adapted procedures to these shortcomings so as to minimize their effect.

The devices of this invention are distinct improvements on separatory funnels and allow for a non-tedious, rapid, and semi-automatic operation. Such benefits become a very distinct advantage when a series of separating funnels are to be operated making a plurality of simultaneous separations. Such multiple separations are conventional in chemical and biochemical research and development.

In chemical and biochemical operations such as solvent extraction, steam distillation, and azeotropic distillation, there are present two immiscible liquids which must be separated from each other at some stage in the process. A very effective method is to use the separatory funnel devices of the present invention. That is, in a liquid - liquid extraction the two liquids may be contacted by agitation, followed by a settling period, followed by a removal of either layer or both layers. The devices of this invention are particularly useful when only the upper layer is to be removed, and the lower layer contacted with fresh solvent. In steam or azeotropic distillations where the distilled product forms two layers, this product can be run into a separatory device of this invention and either or both layers removed batchwise or continuously. Again, the devices of this invention are very particularly beneficial when a plurality of separations are to be made.

Briefly, the devices of this invention comprise a container flask preferably in the shape of a separatory funnel with a conduit means extending upwardly from a low portion of the bottom surface of this container flask. This conduit is adjustable in regards to essentially any position in the vertical height in the container flask, and includes a valve means such as a stopcock at a lower portion of the conduit, preferably below the bottom surface of the container flask. The function of this conduit is to remove at least part of the upper layer of a two layer system. By being able to adjust the vertical height of this conduit, all or part of the upper layer may be removed. Then by lowering this conduit to the region of the bottom of the container flask, the lower layer can be removed. Also, considered a part of this invention is a separate conduit or drain means for removing the lower layer. This can consist of a separate conduit and valve, or may utilize a separate conduit but the same valve as used in removing the upper layer. However, in any embodiment there is provided a rapid and effective method to separate liquid materials which have separated into two distinct layers, and particularly when these layers are liquid layers of significantly different specific gravities.

It is, therefore, a prime object of this invention to set out separatory funnel devices which can effectively remove either the upper or lower layer of a separated liquid mixture in a manner free of any contamination from the remaining layer.

It is, additionally, an object of this invention to disclose separatory funnel devices wherein each layer may be separated utilizing separate conduit means for each layer whereby neither layer is contaminated with liquid from the other layer.

It is, also, an object of this invention to describe separatory funnel devices which can be operated easily and rapidly, and which therefore are very well adapted for use in multiple liquid separations.

These and other objects will be more fully described and explained with reference to the drawings and detailed disclosure of this specification.

FIG. 1 is a front elevational view of a separatory funnel having an adjustable conduit means for removing an upper layer.

FIG. 2 is a front elevational view of a separatory funnel with a slideable adjusting means for the upper layer removing conduit.

FIG. 3 is a front elevational view of a separatory funnel having a separate conduit and valve means for removing a lower liquid layer.

FIG. 4 is a front elevational view of a separatory funnel having a single valve and a drain means for removing the upper or lower liquid layer.

In more detail, FIG. 1 shows a separatory flask container section 10 with a stopper closure 11 at the upper end. At a lower portion 12, the container section connects with a fitted plug 13 having internal threads and is sealed against any leakage by washer 14. Lock nut device 17 holds the lower portion 12 in contact with the washer 14. Threaded conduit 16 passes through the threaded plug 13 and up into the container section of the separatory flask. In the embodiment of this figure, the threaded conduit 16 carries removeable extension tube 15. This extension tube increases the height of the threaded conduit to the region within the container section of the separatory flask where the division of the layers is expected. Fine adjustment to the exact level of the division of the liquids is made by rotating conduit 16 which then via the threaded plug 13 raises or lowers the top of the extension tube 15 which is open. On the lower end of conduit 16 is stopcock valve 18 and a portion 19 which may be threaded so as to accept an extension stem 20. Therefore on adjustment of the conduit 16, with or without extension tube 15 to the appropriate level, followed by the opening of the stopcock valve 18, an upper liquid layer in the container portion of the flask can be rapidly removed.

FIG. 2 discloses an embodiment wherein the separatory flask has a plug 13 in lower portion 12 of the container section of the flask which is not threaded. The conduit 16 is slideably adjustable in plug 13 and is sealed in plug 13 optionally using O-ring 21. The sealing method of the plug to the lower portion of the container is the same as in FIG. 1 as also is the stopcock valve arrangement. In this embodiment, however, the height of the conduit is adjusted by a sliding movement and then locked in position by flair nut 22. After being locked in a position so that the top of conduit is in the upper liquid layer, this upper layer can rapidly be removed. By lowering the conduit, the lower layer can then be removed.

FIG. 3 sets out an embodiment similar to FIG. 1 except that in the lower portion 12 of the flask container, there is provided a separate conduit 23 and stopcock valve 24 for removal of the lower liquid layer. Thus, in this embodiment of the invention the upper layer can be removed via extension tube 15 and stopcock valve 18, and the lower layer removed via conduit 23 and stopcock valve 24.

FIG. 4 illustrates another embodiment of a separatory funnel wherein the same conduit 16 and stopcock valve 18 is utilized for the removal of the upper liquid layer and lower liquid layer. In this embodiment the plug 13 is maintained in the container lower portion 12 by the same means as in FIG. 1. That is, the plug 13 is maintained and sealed in lower portion 12 by washer 14 and lock nut 17. The conduit 16 is slideably adjustable in plug 13 and may optionally contain an O-ring seal 21. If an O-ring seal is not used, the conduit 16 should be of a close fit in plug 13. In the lower part of conduit 16 within plug 13, there is a drainage hole 25 which is brought into alignment with plug drain hole 26 when it is desired to remove a lower liquid layer. When not in alignment, the upper liquid layer can be removed. This alignment is accomplished by removing the disc lock washer 28, moving the conduit 16 upwardly until the flair nuts 29 and 27 meet and then rotating conduit 16.

The operation of these separatory funnels is self explanatory; however, an extraction using the separatory funnel of FIG. 4 will be described. When sodium acetate is contacted with an aqueous sulfuric acid solution, there results a comixture of acetic acid, water and sodium sulfate. The acetic acid can be separated by extraction with butyl acetate, ethyl ether or methyl isobutyl ketone. In this example, ethyl ether will be used. The comixture is added to the flask container section and an equal volume of ethyl ether is added. The flask is stoppered, agitated, followed by a short period for formation of an aqueous layer and acetic acid laden ethyl ether layer. The ethyl ether layer is the upper layer. During this procedure, the drain holes 25 and 26 are in a non-alignment. The flair nut 27 is then loosened and the height of the conduit 16 adjusted to the level of the ethyl ether layer. Flair nut 27 is then tightened to maintain this adjustment. The upper acetic acid laden ethyl ether layer is then removed via stopcock 18. A second portion of ethyl ether equal in volume to the first portion is added and the procedure repeated. This also forms an upper layer and lower layer. This upper layer is removed via stopcock 18 and combined with the first extracted portion. The acetic acid and ethyl ether can be separated by distillations.

The aqueous lower layer is removed from the flask by aligning drain holes 25 and 26 and draining via stopcock 18. This alignment is accomplished by manipulation of flair nuts 27 and 29 and lock washer 28.

The separatory devices of this invention may be constructed using many suitable materials. These include glass, metals or metal alloys or plastics. Preferably, the flask container portion is glass or plastic with the conduit, plug and stopcock valve being plastic. Very suitable plastics are teflon, nylon, polyethylene, polypropylene and polystyrene. Other plastics, however, may also be used and are considered to be within the scope of this invention.

Claims

I claim:

1. A liquid separating device comprising a flask container; a conduit passing through the lower surface of said flask container and adjustably extending up into said flask container to a set height; and a conduit height adjusting means and valve means on the portion of said conduit below said lower surface of said flask container.

2. A device as in claim 1 wherein said conduit height adjusting means comprises a threaded portion on said conduit which engages and passes through a plug seal in the bottom surface of the flask container whereby on rotation of said conduit, the height of said conduit within said container flask is changed.

3. A device as in claim 2 wherein on a portion of said conduit below said flask container, there is a locking means whereby said conduit is maintained in the adjusted height.

4. A device as in claim 2 wherein a second conduit extends from the lower portion of said flask container, said second conduit having a valve means whereby a lower liquid layer in said flask container can be selectively removed.

5. A device as in claim 2 wherein said conduit and said plug seal each have a drain aperture, the conduit drain aperture being alignable with the plug seal drain aperture whereby a lower liquid layer in said flask container can be selectively removed.

6. A device as in claim 5 wherein said conduit drain aperture is maintained in alignment with said plug seal drain aperture by a conduit locking means.

7. A device as in claim 1 wherein said conduit height adjusting means comprises a portion on said conduit which closely engages and passes through a plug seal in the bottom surface of the flask container whereby said conduit can be slideably moved within said plug seal thereby effecting the height adjustment of said conduit.

8. A device as in claim 7 wherein on a portion of said container below said flask container, there is a locking means whereby said conduit is maintained in the adjusted height.

9. A device as in claim 7 wherein a second conduit extends from the lower portion of said flask container, said second conduit having a valve means whereby a lower liquid layer in said flask container can be selectively removed.

10. A device as in claim 7 wherein said conduit and said plug seal each have a drain aperture, the conduit drain aperture being alignable with the plug seal drain aperture whereby a lower liquid layer in said flask container can be selectively removed.

11. A device as in claim 10 wherein said conduit drain aperture is maintained in alignment with said plug seal drain aperture by a conduit locking means.