Method and installation for regulating the modifier level in chromatography or supercritical extraction with recycling

• US 8,236,179 B2
• Filed: 11/11/2011
• Issued: 08/07/2012
• Est. Priority Date: 08/12/2005
• Status: Active Grant

• Current Assignee: PIC Solution
• Original Assignee: PIC Solution
• Inventors: Shaimi, Mohamed
• Primary Examiner(s): Therkorn, Ernest G
• Application Number:
  US13/294,565
• Publication Number:
  US 20120055876A1
• Time in Patent Office: 270 Days
• Field of Search: 210/635, 210/656, 210/659, 210/101, 210/137, 210/143, 210/198.2, 961/02, 95/82
• US Class Current: 210/659
• CPC Class Codes: B01D 15/166 Fluid composition conditioning, e.g. gradient
• CPC Class Codes: B01D 15/1814 recycling of the fraction to be distributed
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent

Abstract

A chromatography or supercritical extraction method is disclosed, in which the eluent comprises a mixture of a fluid and a modifier and in which the fluid is recycled. One exemplary method comprises an operation consisting in determining at least one quantity linked to the level of modifier that is mixed with the recycled fluid and, if necessary, a correction operation in order to limit variations in the level of modifier in the eluent at the inlet of the column or the extractor. The disclosure also relates to a chromatography or extraction installation.

Claims

1. A separation method, including:

performing a separating operation in a separation device, with the separation device receiving a product and feeding into an eluent that includes a supercritical fluid, routed via a first pumping operation, and a modifier, routed via at least one second pumping operation,

collecting at least one fraction of the product downstream of the separation device,

recycling the supercritical fluid mixed with a residual quantity of modifier, following after the collecting operation and preceding the first pumping operation, with the first pumping operation being used to pump at least the supercritical fluid mixed with a residual quantity of modifier, and

performing a condensing operation following after the collecting operation and preceding the first pumping operation,

the method being characterised in that it further includes;

downstream of the collecting operation and upstream of the separating operation, determining at least one magnitude associated with the level of modifier mixed with the recycled supercritical fluid, and if necessary

correcting the flow in the first pumping operation and the flow in the second pumping operation, in order to limit the variations, during execution of the method, of the modifier level in the eluent at the input to the separation device, in a direction that is suitable for meeting a first setpoint, determined beforehand, for the total flow.

2. The method according to claim 1, wherein determining at least one magnitude associated with the level of modifier mixed with the recycled supercritical fluid takes place upstream of the first and second pumping operations and includes:

measuring, at one measuring point at least, the density of the recycled supercritical fluid mixed with a residual quantity of modifier, and

evaluating the level of modifier mixed with the recycled supercritical fluid, with the modifier level being evaluated, from the measured density, by means of a density=f (modifier level) calibration curve, established beforehand at the pressure and the temperature existing at the measuring point and around the latter; and

wherein the correcting operation consists of modifying the flow in the first pumping operation and the flow in the second pumping operation in order to meet the first setpoint and a second setpoint, set beforehand, of levels of modifier in the eluent.

3. The method according to claim 2, wherein the first pumping operation and the second pumping operation take place in parallel with each other.

4. The method according to claim 2, wherein the second pumping operation takes place upstream of the first pumping operation.

5. The method according to claim 1, wherein determining a magnitude associated with the modifier level in the eluent consists of measuring the density of the eluent upstream of the first pumping operation and downstream of the second pumping operation, and

wherein the correcting operation consists of modifying the flow in the first pumping operation and the flow in the second pumping operation in a direction that is suitable to attain the first setpoint and a third setpoint, set beforehand, for the density of the eluent.

6. The method according to claim 1, wherein determining at least one magnitude associated with the level of modifier mixed with the recycled supercritical fluid is effected downstream of the condensing operation.

7. The method according to claim 1, wherein determining at least one magnitude associated with the level of modifier mixed with the recycled supercritical fluid is effected upstream of the condensing operation.

8. The method according to claim 1, wherein the supercritical fluid is carbon dioxide.

9. The method according to claim 1, wherein the modifier is an organic liquid solvent, like an alcohol for example.

10. The method according to claim 1, further including regulating the pressure followed by regulating the temperature, downstream of the separating operation and upstream of the collecting operation.