Liquid purification or separation – Processes – Chromatography
Reexamination Certificate
1999-12-30
2001-11-06
Therkorn, Ernest G. (Department: 1723)
Liquid purification or separation
Processes
Chromatography
C210S659000, C210S198200
Reexamination Certificate
active
06312603
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus for separating two or more components existent in a solvent for chromatography by combining multiple powder containers filled with multiple stationary phase powders for chromatography with multiple solvent container filled with the solvent for chromatography, and to a method using the apparatus.
2. Description of the Related Art
For the separation of a large amount of an organic compound that is difficult to be purified in large quantities by fractional distillation or fractional crystallization, there is liquid chromatography making use of a difference in partition factor between the solid phase and the liquid phase of an organic compound. This involves such economical problems that it requires a large amount of an expensive stationary-phase carrier and the recovery of a large amount of an elute. There is also fluidized stationary phase chromatography in which a stationary phase is added continuously to cause a liquid phase and the stationary phase to flow countercurrently to each other unlike general chromatography. This is conceptually possible but it is difficult to put it into practice.
In the case of separation by liquid chromatography, an elute generally moves and the length that the elute moves and reaches partition equilibrium is considered as one stage. Since the elute reaches equilibrium while moving, in the case of a column for preparation having a large diameter, the effective number of stages per the length of the column tends to be small.
SUMMARY OF THE INVENTION
The present invention relates to a separating apparatus for carrying out (m+n)-stage solid-liquid countercurrent extraction many times continuously, the apparatus comprising:
a row of (m+n) powder containers filled with stationary phase powders for chromatography, a new powder container being able to be added adjacent to the right side of a first powder container from the right of the row and a (m+n)-th powder container from the right being able to be removed simultaneously with, before or after the addition of the new powder container;
a row of (m+n) solvent containers filled with a solvent, a new solvent container being able to be added adjacent to the left side of a (m+n)-th solvent container from the right of the row and a first solvent container from the right of the row being able to be removed simultaneously with, before or after the addition of the new solvent container;
a sample feed device for supplying a sample solution consisting of the same solvent as the above solvent and two or more components to be separated to an m-th solvent container from the right of the row of the solvent containers;
a powder container feed device for supplying the new powder container to the right end of the row of the powder containers;
a powder container removing device for removing a powder container from the left end of the row of the powder containers;
a solvent container feed device for supplying the new solvent container to the left end of the row of the solvent containers; and
a solvent container removing device for removing a solvent container in which the sample components have been separated from the right end of the row of the solvent containers, wherein
the apparatus repeats the following stages (a), (b), (c) and (d) a required number of times,
and to use of the apparatus making use of separation conditions obtained by the computer simulation of the following numerical expression 1;
(a) a stage in which the sample solution is supplied to the m-th solvent container from the right for the first solid-liquid partition for the (m+n)-stage countercurrent extraction of the sample components, the powders and the solvent are mixed and stirred by pairing and coupling all the powder containers and the solvent containers of the same numbers from the right in the rows with each other, when partition equilibrium between solid phase and liquid phase by contact between the solvent and the powders in each of the paired powder containers is attained, the powders and the solvent in each of the paired powder containers are separated from each other and the solvent is returned to its solvent containers, and the two interconnected rows are separated from each other to complete the first (m+n)-stage partition between solid phase and liquid phase;
(b) a stage in which the row of the above powder containers moves to the left by one stage, one new powder container is added to the right end of the row of the powder containers, and a powder container in which sample components have been separated is removed from the left end of the row of the powder containers, thereby forming a new row of (m+n) powder containers;
(c) a stage in which after the above sample solution is supplied to the m-th solvent container from the right for second solid-liquid partition for the (m+n)-stage countercurrent extraction of the above sample components or without supplying the sample solution, the powders and the solvent are mixed and stirred by pairing and coupling the powder containers and the solvent containers of the same container numbers from the right in the rows with each other, when partition equilibrium between solid phase and liquid phase by contact between the solvent and the powders in each of the paired powder containers is attained, the powders and the solvent in each of the paired powder containers are separated from each other and the solvent is returned to its solvent containers, and the two interconnected rows are separated from each other to complete the second (m+n)-stage partition between solid phase and liquid phase; and
(d) a stage in which the row of the solvent containers moves to the right by one stage, one new solvent container is added to the left end of the row of the solvent containers, and a solvent container in which sample components have been separated is removed from the right end of the row of the solvent containers, thereby forming a new row of (m+n) solvent containers.
The expression “solid-liquid countercurrent extraction” means that the solid phase and the liquid phase of chromatography are contacted to each other by causing them to flow countercurrently to each other to adsorb part of the components contained in the liquid phase to the solid phase and simultaneously extract part of the components adsorbed to the solid phase into the liquid phase for the partition of these components between the solid phase and liquid phase (partition (equilibrium) of components between solid phase and liquid phase will be referred to as “partition (equilibrium) between solid phase and liquid phase” or “partition (equilibrium)” hereinafter).
The apparatus of the present invention is aimed to carry out this “partition between solid phase and liquid phase” not between a solid phase and a liquid phase which are caused to flow countercurrently to each other continuously but between a solid phase and a liquid phase which are caused to flow countercurrently to each other intermittently by partitioning among (m+n) pairs of separate containers arranged in a row. Since a liquid can be caused to stay in the containers until partition equilibrium which is preferred from a practical point of view is attained by partitioning among separate containers, the partition efficiency in each separate container is increased.
In the countercurrent extraction of the present invention, the solid phase and the liquid phase move in opposite directions as a matter of course. The expression “(m+n) stage countercurrent extraction between solid phase and liquid phase” in the present invention means that partition equilibrium in the above (m+n) pairs of separate containers, separation between solid phase and liquid phase, the disconnection of the pair and the movement of the next liquid phase (for the formation of new pairs with the solid phase of the pair at a downstream) are carried out among each pair simultaneously or almost simultaneously.
Separate containers are divided into powder co
Oliff & Berridg,e PLC
Therkorn Ernest G.
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