Patent Application
20230124541
This invention relates to devices and methods for liquid separation.
In routine chemical and biochemical processes, such as solvent extraction, steam distillation and azeotropic distillation, immiscible liquids, usually an organic soluble liquid and an aqueous soluble liquid, must often be separated from each other by separatory funnels. In liquid--liquid extractions, liquids may be contacted by agitation, followed by a settling period, followed by removal of one or more layers of liquid.
In typical synthetic procedures, the reaction mixtures need a workup process as follows: the reaction mixtures are distributed between an organic and aqueous layer, then the organic layer is separated and transferred to an Erlenmeyer flask. Next, desiccants, such as sodium sulphate, magnesium sulphate, or other desiccants, are put into the Erlenmeyer flask. After a period of time, such as thirty minutes, the desiccants are filtered off by filter funnels. So a dry and transparent solution is obtained, which will be concentrated and further purified to get the target compounds.
The present invention, in at least one embodiment, relates to an apparatus for a combined function of regular separatory funnels, Erlenmeyer flasks for drying liquid, and filter funnels. An apparatus, of at least one embodiment of the present invention, also reduces the workup time of a chemical process, which uses the same apparatus for liquid separation, drying and filtration. In at least one embodiment, a method for separating immiscible liquids from insoluble solids is also provided.
At least one embodiment of the present invention provides a novel separatory funnel, which reduces the amount of time necessary for funneling, drying, and filtering of liquids. This novel separatory funnel has the functions of a regular separatory funnel, Erlenmeyer flask and filter funnel. The usage of this funnel also eliminates the need for extra glassware, such as Erlenmeyer flask and filter funnel.
To achieve the foregoing solutions and in accordance with the purpose of one or more embodiments of the present invention, there is provided a separatory funnel comprising: a chamber having an inlet opening and an outlet opening for allowing a liquid to flow through the chamber; and a horizontally aligned filter plate disposed between the inlet opening and the outlet opening along the longitudinal axis of said chamber, said filter plate positioned such that the periphery of said filter plate is placed, stuck, and/or sealed directly to the interior wall of said chamber. The said filter plate is positioned between the inlet opening and the outlet opening, so the liquids are filtered and solids or precipitates are kept in the funnel, and clear liquid phases are obtained as either combined or separated phases .
Further in accordance with the purposes of the present invention as embodied and broadly described herein, there is provided a method for separating at least two immiscible liquids in a mixture, and then dry and filter the organic layer in one glassware, comprising the steps of: pouring the mixture through a transparent chamber having an inlet opening and an outlet opening for allowing the liquids to flow through the chamber; allowing the mixture to form at least one distinguishable interface between a lower layer of one liquid and an upper layer of another liquid; allowing the mixture to flow through a passage formed by a horizontally aligned filter plate disposed in the chamber such that at least a portion of the periphery of said baffle plate is placed directly against the interior wall of said chamber, until the one liquid has exited from said chamber leaving the liquid in the upper layer in the chamber; and regulating the flow of the one liquid in the lower layer from the chamber to separate the liquids. The upper layer, usually an organic phase, such as ethyl acetate, diethyl ether, hexane or other organic solutions, is kept in an inner chamber of the apparatus. Then desiccants, such as sodium sulphate, or magnesium sulphate, or other desiccants, are put into the inner chamber of the apparatus. The said apparatus is then shaked, swirled or flipped for a few times to let the liquid interact with desiccants. Next an outlet valve is opened to allow the mixture to flow through the filter plate, and out an outlet opening, so a transparent liquid free from water or moisture is obtained.
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate the presently preferred embodiments of the present invention and, together with the general description given above and the detailed description of the preferred embodiments given below, serve to explain the principles of the invention.
Reference will now be made in detail to the present preferred embodiments of the invention as illustrated in the accompanying drawings.
The apparatus 1 is a combination of a known separatory funnel device 2 and a filter 4 placed within an inner chamber 2b of the known separatory funnel device 2.
The present invention, in at least one embodiment, provides the apparatus 1 of
The known separatory funnel device 2 is comprised of an inlet opening 2a and an outlet opening 2e. The outlet opening 2e allows a liquid to flow through an inner chamber 2b. The inner chamber 2b is enclosed within an outer housing 2c, which may be made of glass. The known separatory funnel or funnel device 2 may be a known cylindrical, substantially cylindrical, or tapered cylindrical known separatory funnel device 2.
Preferably, the inner chamber 2b is wide, and may have a diameter of D2, following entrance through inlet opening 2a and tapers to a relatively narrow outlet opening 2e. In a preferred embodiment, the inner chamber 2b comprises a funnel, such as a pouring funnel or a separatory funnel. Inlet opening 2a, provided near the upper end of inner chamber 2b, may be wide as in conventional pouring funnels or relatively smaller as in separatory funnels. For example, in a five hundred ml (milliliters) separatory funnel, inlet opening for opening 2a may be about 11/8 inches in diameter D1, and may be fitted with a stopper or other type of closure to keep the mixtures inside the funnel while operating.
As shown in
Filter plate 4 is positioned such that at least a portion of the periphery of the filter plate 4 is placed directly against an interior wall of the housing 2c, and forms a porous passage for the flow of liquid therethrough. Filter plate 4 completely covers the space directly above outlet opening 2e as viewed along the longitudinal axis of the inner chamber 2b.
The apparatus of the present invention may further include means for regulating the flow of liquid from inner chamber 2b. The regulating means may comprise a variety of valves, such as a check valve or a stopcock, such as valve 2d shown in
In a preferred embodiment, filter plate 4 is placed low in the inner chamber 2b such that it is positioned along the longitudinal axis of inner chamber 2b such that the distance as measured along the longitudinal axis from the regulating means 2d to the filter plate 4 is less than 1/5 of the distance measured along the longitudinal axis from the regulating means 2d to inlet opening 2a. For example, in a 500.0 (five hundred) ml (milliliters) separatory funnel 2, filter plate 4 will typically be positioned about 0.5 inches above the stopcock or valve 2d. Filter plate 4, as shown in
The apparatus 1 of
The filter plate 4 may be positioned such that a periphery of said filter plate 4 is placed, stuck, or sealed directly to an interior wall of the housing 2c for the inner chamber 2b. The said filter plate 4 is typically positioned between the inlet opening 2a and the outlet opening 2e, so the liquids are filtered and solids or precipitates are kept in the funnel, in the upper layer 3a, or the area in the inner chamber 2b between inlet opening 2a and the filter 4, and clear liquid phases are obtained passing through the filter 4 into the lower layer 3b, through the outlet 2e as either combined or separated phases. The filter 4 divides the inner chamber 2b into the upper layer 3a and the lower layer 3b. The filter 4 has a three hundred sixty degree periphery which surrounds and delimits the filter 4 and which is in contact with a three hundred sixty degree inner wall of the housing 2c, so that material typically must go through the filter 4 in order to pass from the upper layer 3a into the lower layer 3b.
The filter plate 4 may be a fritted glass plate or other porous membrane, which can filter liquid. The filter plate 4 may be positioned along the longitudinal axis of the inner chamber 2b such that filter plate 4 is near or close to the outlet opening 2e.
In at least one embodiment, a method is provided for separating at least two immiscible liquids in a mixture, comprising the steps of:
Although the invention has been described by reference to particular illustrative embodiments thereof, many changes and modifications of the invention may become apparent to those skilled in the art without departing from the spirit and scope of the invention. It is therefore intended to include within this patent all such changes and modifications as may reasonably and properly be included within the scope of the present invention’s contribution to the art.
