Source: http://www.google.com/patents/US6475392?dq=5,973,252
Timestamp: 2016-10-25 15:51:57
Document Index: 391443493

Matched Legal Cases: ['art 1', 'art 2', 'art 1', 'art 2', 'art 1', 'art 2', 'art 2', 'art 1', 'art 1', 'art 1', 'art 2']

Patent US6475392 - Multistage liquid-solid fractional extraction apparatus - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsThe object is to provide a multistage liquid-solid fractional extraction apparatus in which a separation procedure of a large amount of mixture can be carried out exactly and effectively in a simple procedure by use of a partition difference in liquid chromatography. The multistage liquid-solid fractional...http://www.google.com/patents/US6475392?utm_source=gb-gplus-sharePatent US6475392 - Multistage liquid-solid fractional extraction apparatusAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS6475392 B2Publication typeGrantApplication numberUS 09/792,355Publication dateNov 5, 2002Filing dateFeb 23, 2001Priority dateJul 30, 1998Fee statusLapsedAlso published asUS6224761, US20010030155Publication number09792355, 792355, US 6475392 B2, US 6475392B2, US-B2-6475392, US6475392 B2, US6475392B2InventorsTakenori TanimuraOriginal AssigneeTakenori TanimuraExport CitationBiBTeX, EndNote, RefManPatent Citations (13), Non-Patent Citations (1), Referenced by (7), Classifications (14), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetMultistage liquid-solid fractional extraction apparatus
US 6475392 B2Abstract
The object is to provide a multistage liquid-solid fractional extraction apparatus in which a separation procedure of a large amount of mixture can be carried out exactly and effectively in a simple procedure by use of a partition difference in liquid chromatography. The multistage liquid-solid fractional extraction apparatus comprises multiple containers 3 capable of accommodating liquid and solid for a liquid-solid extraction, a liquid inlet part 1 and a liquid outlet part 2 equipped with in each container, a pipe 4 to carry liquid from the liquid outlet part of the forward container to the liquid inlet part of the backward container, an efflux protecting device (filter 5) for solid, which is equipped with at the above liquid outlet part, and along with these a stirring device to let solid in said container move in liquid by virtue of the density difference between solid and liquid when rotating or swinging the container 3. Images(5) Claims(3)
What is claimed is: 1. A multistage liquid-solid fractional extraction process comprising the step of:
extracting a mixture with a multistage liquid-solid fractional extraction apparatus comprising a plurality of containers containing liquids and solids for separating the components of the mixture, wherein the uptown direction of the containers is changed during the extracting step resulting in the solids moving within the liquids by virtue of a density difference between the solids and liquids, and wherein the up-down direction of the container is changed by swinging the container. 2. The multistage liquid-solid fractional extraction process of claim 1, wherein the up-down direction of the container is changed to uniformly mix the liquids and solids.
3. The multistage liquid-solid fractional extraction process of claim 1, wherein the apparatus comprises:
(a) multiple containers capable of accommodating liquids and solids subjected to a liquid-solid fractional extraction, each container having a liquid inlet part and a liquid outlet part; (b) a carrying device to carry the liquid from the liquid outlet part of one container to the liquid inlet part of another container; and (c) a stirring device to change the up-down direction of the containers, such that the solids within the liquid in the containers move by virtue of a density difference between the solids and liquid, wherein at least one liquid outlet part comprises an efflux protecting device for preventing solids from flowing out of the container, and wherein the stirring device is capable of swinging the containers.
This is a, divisional of application Ser. No. 09/360,982, filed Jul. 26, 1999, now U.S. Pat. No. 6,224,761. The prior applications is hereby incorporated herein by reference, in its entirety.
As a method to remove or to recover a substance in solution by means of its adsorption to solid, a decoloration by the active carbon, a removal of the ion by the ion-exchange polymer or the like are widely known. These procedures mostly finish in one step, however in case of separating each kind of substances by making use of the difference in each adsorption power to a specific solid, the chromatography is widely used. The chromatography is a technology in which a fine solid in a uniform shape is packed in the column, liquid or gas as a mobile phase is flowed therein, and a lot of substances existing in a solution or gas are separated by making use of a distribution difference of substances in between solid and liquid or between solid and gas, and is an extremely effective device which can carry out a mutual separation by making use of as mall difference of the distribution coefficients in case of the separation of a small amount of mixture.
FIG. 1 is the rough figure showing one example of embodiments of the multistage liquid-solid fractional extraction apparatus according to the invention. One constitutional unit of the multistage liquid-solid fractional extraction apparatus is a sealable container 3 having the inlet part 1 and the outlet part 2 of the liquid as a mobile phase, and the multistage liquid-solid fractional extraction apparatus is constructed by connecting the liquid inlet part 1 and the liquid outlet part 2 of a lot of containers 3 by the pipe 4 which is a carring device of liquid. In the outlet part 2 of liquid, for example, a mesh type filter 5 is provided as an efflux protecting means to protect solid in the container 3 for flowing out together with liquid. Further, it is not necessary to provide a filter at the liquid inlet part 1, but it is possible to exclude the directivity of the container 3 by providing the same filter at the inlet part 1 as well.
As shown in FIG. 2 and FIG. 3, a plurality of containers 3 are respectively set up to the stand 6 which holds and can rotate or swing the containers, and each container is connected in series by the pipe 4. The containers 3 are rotated or swinged at an appropriate speed in connection with the axis 6 a of this stand 6 to a driving device such as a motor or a crank, so that solid in the container moves in liquid by virture of the density difference from liquid, accelerating a substance equilibrium partition between solid and liquid.
Each container 3 is filled with e.g. an appropriate amount of adsorbent as a solid, and a liquid as a mobile phase and then sealed. When a mobile phase solution is supplied at an optional amount of flow from the liquid inlet part 1 of the starting container while rotating or swinging the container 3 at this state, a volume of liquid corresponding to a liquid amount supplied flows out from the liquid outlet part 2. At this time, the amount of substance existing in the liquid flowing out of the container 3 is expected to be in a partition equilibrium state against the adsorbent. Therefore, in an ideal case, one container 3 corresponds to one plate in the plate theory of the chromatography. Accordingly, e.g. 10 pieces of containers are connected, a separation system corresponding to 10 plates of the chromatography is to be formed as a matter of course.
On the other hand, a column having theoretical plates exceeding several thousands of plates is as a rule used in chromatography, and also, the above-menionted multistage liquid-solid fractional extraction apparatus needs several thousands of containers because containers corresponding to at least theoretical plates must be connected.
For example, considering Gauss distribution, if an aimed component in the initial sample is taken in about 98% yield, the separation efficiency of that system is to have 100 plates compared to the number of theoretical plates of chromatography. If 6 units are made by 120 containers of two times, the separation efficiency of the system becomes 400 plates, and it: becomes 10,000 plates if tenfold containers are used.
Further, in case of carrying out separation of a racemate, in the center part of the peak of two optical antipodes, there is always a part in which the optical antipodes exist in the same amount, and therefore if it is possible to confirm this part by analysis, it is also possible to carry out. automatically the addition of an sample because a racemate which becomes a new resolution object can be added to that part.
A medicine bottle of inner volume 25 ml, manufactured by Iwaki Glass Co., Ltd., was used as a container. To this container was connected two tubes of inner diameter 1 mm, whereby the one was made the inlet part of the mobile phase (liquid), and the other was made the outlet part of the mobile phase (liquid) equipped with filter. 2 g of Amberlite XAD4 (trade name) was introduced into each container as solid for adsorption (adsorbent), and it was packed with 70% methanol as liquid for extraction (extraction liquid) and sealed. This type of 40 containers were prepared, and the inlet part and the outlet part were successively connected in series, followed by installing them to the rotatory stand.
Being associated with rotation of the rotary stand at about 60 rotation/min., the first container was filledd with 70% methanolic solution 2 ml containing ethyl p-hydroxybenzoate (concentration 30 g/l) and butyl p-hydroxybenzoate (concentration 60 g/l), followed by starting the extraction by passing 70% methanol at flow rate 4 ml/min. from the side of the first container. During the operation, it was observed in the container that the adsorbent moved in the extraction liquid by subsidence accompanying the change of the up-down direction of the container by rotation.
The elute from the 40th container was fractionated at every 200 ml by use of the fraction collector, and ethyl p-hydroxybenzoate and butyl p-hydroxybenzoate in each fraction where quantified by high pressure liquid chromatography (HPLC). The result is shown in FIG. 4. As is evident from this result, it can be understood that each container corresponds to about one plate of the theoretical plate number of chromatography.
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