EP1379867A1 - Schutzeinrichtung für das chromatographische bett in dynamischen axialkompressionschromatographiesäulen - Google Patents

Schutzeinrichtung für das chromatographische bett in dynamischen axialkompressionschromatographiesäulen

Info

Publication number
EP1379867A1
EP1379867A1 EP02761925A EP02761925A EP1379867A1 EP 1379867 A1 EP1379867 A1 EP 1379867A1 EP 02761925 A EP02761925 A EP 02761925A EP 02761925 A EP02761925 A EP 02761925A EP 1379867 A1 EP1379867 A1 EP 1379867A1
Authority
EP
European Patent Office
Prior art keywords
bed
pressure
fluid
piston
column
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP02761925A
Other languages
English (en)
French (fr)
Inventor
Wilhelm Hauck
Harlene Marks
Jean Blehaut
Roger-Marc Nicoud
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Novasep Process SAS
Original Assignee
Novasep SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Novasep SAS filed Critical Novasep SAS
Publication of EP1379867A1 publication Critical patent/EP1379867A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1809—Controlling processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces
    • G01N30/6021—Adjustable pistons
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid
    • G01N30/52—Physical parameters
    • G01N2030/522—Physical parameters pressure
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces

Definitions

  • the present invention relates to the protection of the chromatographic bed of chromatographic columns and in particular in columns with dynamic axial compression.
  • the column is generally filled with a solid product in the form of very fine grains, usually between 5 and 100 ⁇ m in size, forming the chromatographic bed.
  • the arrangement of the grains inside the column must be as homogeneous as possible and, moreover, empty volumes must be avoided between the chromatographic bed and the inputs-outputs of the column. It is known in the prior art to use columns with dynamic axial compression in order to ensure the existence of a compact bed, with no free space between the inlet-outlet distributors and the bed.
  • a chromatography device in the form of a column intended to contain a bed of adsorbent material.
  • the apparatus consists of a tube comprising a cover and a body sliding in the tube for exerting pressure in the tube.
  • the sliding body is a piston comprising at its head a porous plate permeable to fluids.
  • a suspension of particles of a material capable of constituting an adsorbent bed is introduced into the tube devoid of its cover, the piston being set back enough to allow the introduction of the suspension, without being necessarily in neutral.
  • the cover is adapted to the tube, then pressure is exerted on said suspension by means of the piston.
  • the liquid is discharged through the porous plates, and said particles are compressed between the piston and the cover.
  • This device makes it possible, in an exemplary embodiment, to reach the stage of compression of the bed chosen and the settlement of the particles desired when the sliding body has traveled 2/5 of the height of the column.
  • this device has the disadvantage of achieving imprecise settlement of the bed, since it is evaluated by the sole position of the piston along the tube.
  • a chromatography apparatus comprising a tube of which a part is intended for contain an adsorbent bed.
  • This tube has two end walls and a piston sliding longitudinally in the tube.
  • the piston marks between the two end walls a separation between a chamber chromatography containing the bed and an enclosure in which a pressure prevails so as to move the piston along the tube.
  • the particularity of this device is that the fluid contained in the enclosure is liquid to be chromatographed derived from the inlet pipe thereof.
  • a part of the liquid is diverted towards the enclosure by an enclosure conduit and the other part of the liquid is entrained towards the chromatographic chamber by a flow conduit passing through the enclosure and the piston.
  • the force exerted on the side of the enclosure on the piston is equal to the sum of the force on the piston caused by the flow of the liquid in the chamber to be chromatographed and the mechanical force of the bed on the piston.
  • This device allows, in addition to performing the elution step, to define the pressure exerted on the bed.
  • the piston has a constant cross-section but the pressure in the flow and enclosure conduits is regulated by pressure reducing valves.
  • the tabs can be tared so that the difference in pressures exerted by the flow of the liquid and by the liquid in the enclosure is adjusted to a set pressure on the bed.
  • the pressure in the flow and enclosure conduits is the same but the cross section of the piston varies.
  • the piston has two sections sliding in corresponding bores, the smallest section A being located on the side of the chromatographic chamber and the largest section B on the side of the enclosure. Due to the difference in surface area of the faces A and B of the piston, the force exerted at B is greater than the force exerted at A.
  • the sections of the piston can be chosen so that the difference in pressures exerted by the flow of the liquid and by the liquid in the enclosure is adjusted to a set pressure on the bed.
  • the apparatus described in the above document has various drawbacks. If a pressure drop occurs in the flow conduit, the pressure exerted on the piston by the liquid in the enclosure applies directly to the bed which can cause deterioration of the bed. In addition, the movements of the chromatographic bed not being monitored and the enclosure being unable to discharge liquid during the chromatography, this device cannot adapt the pressure exerted on the bed as a function of the movements of the latter. A deterioration of the bed can again follow. On the other hand, this system cannot be used in SMB (Simulated Moving Bed) or in NARICOL. In such configurations, the chromatography devices are mounted in a loop and the liquids injected into the beds alternate. In the apparatus described in EP-A-0 145 578, the same liquid is sent into the bed and into the enclosure, the alternation of injection of liquids generates a mixture of these.
  • SMB Simulated Moving Bed
  • the present invention relates to an improved chromatography device which overcomes the drawbacks of known devices. This device increases the efficiency of the chromatographic bed while protecting it.
  • the present invention relates to a chromatography device comprising:
  • the regulator is Integral Proportional Action (PI), Differential Proportional Action (PD) or Differential Integral Proportional Action (PID).
  • PI Integral Proportional Action
  • PD Differential Proportional Action
  • PID Differential Integral Proportional Action
  • the device further includes a first sensor which measures the flow pressure of the first fluid at the inlet of the column and a second sensor which measures the pressure in the chamber.
  • the first fluid flows through the bed from the piston towards the end of the column.
  • the first fluid flows through the bed from the end of the column towards the piston.
  • the piston sliding in the column is connected to another piston sliding in the chamber by a rod.
  • the second fluid is regulated by bypass by the regulator.
  • the invention also provides a set of devices as described above, associated in a loop.
  • the invention also relates to a method for separating at least two compounds from a first fluid, comprising the chromatography of said fluid in the device described above, the method comprises the steps:
  • the invention also relates to a method for adjusting the pressure on the chromatographic bed in the device described above, the method comprising the step:
  • FIG. 1 schematically represents a chromatography device 10 comprising a column 12 for performing the chromatography and a part of which is intended to contain a chromatographic bed 14 resting on an end wall 16.
  • the device 10 also comprises a jack 22.
  • the jack 22 comprises a movable piston 24 connected to one end of a rod 26.
  • the piston 24 delimits two chambers 28 and 30 in the jack 22.
  • the first chamber 28, or upper chamber is delimited between the piston 24 and the upper wall 32 of the cylinder 22.
  • the second chamber 30, or lower chamber is delimited between the piston 24 and the lower wall 34 of the cylinder 22.
  • the lower wall 34 marks the separation between the cylinder 22 and the column 12.
  • the rod 26 connected to the piston 24 is located in the lower chamber 30 and opens into the column 12 passing through the lower wall 34 of the jack 22. Appropriate seals will be used. ilises to seal between the chamber 30 and the column 12.
  • the other end of the rod 26 located in the column 12 is connected to a body 36.
  • the body 36 slides in the column 12.
  • the sliding body 36 is for example a piston. It comes to bear on the chromatographic bed 14.
  • the position of the actuator 22 relative to the column 12 is not limited to that described above. It is in fact possible to envisage placing the jack under the column so that the piston 36 is pressed upwards against the bed 14.
  • the liquid to be chromatographed is conveyed to the bed 14 and is discharged therefrom via flexible communication lines to the outside.
  • the piston 36 includes a conduit 20 provided with a first flow pressure sensor 45.
  • the wall 16 also has a conduit 18.
  • the liquid to be chromatographed reaches the bed 14 via the conduit 20 and then leaves via the of the conduit 18, after passing through the bed 14.
  • the sensor 45 makes it possible to measure the flow pressure of the fluid at the inlet of the column 12.
  • the liquid to be chromatographed can also circulate in the other direction. It then reaches the column 12 via the conduit 18, flows through the bed 14, then leaves the column 12 through the conduit 20.
  • the sensor 45 is placed on the inlet conduit 18.
  • the jack 22 is supplied by a propellant fluid circuit.
  • the cylinder 22 is a double-acting hydraulic cylinder.
  • the propellant fluid is then a hydraulic liquid.
  • a first conduit 38 connects the chamber 28 with a source of hydraulic fluid 44.
  • the conduit 38 includes a second pressure sensor 46.
  • a second conduit 40 connects the lower chamber 30 with the source of hydraulic fluid 44.
  • a conduit bypass 42 connects the conduits 38 and 40.
  • the bypass conduit 42 includes means for regulating the flow of propellant in the bypass. These means include an all or nothing valve (TOR) 48 and a regulation valve 50.
  • the regulation valve is controlled by a regulator 52 of the type with integral proportional action (PI), with differential proportional action (PD) or with proportional action. Differential Integral (PID).
  • PI integral proportional action
  • PD differential proportional action
  • PID Differential Integral
  • the liquids used in the device are separate fluids.
  • the first fluid that is to say the gas or the liquid to be chromatographed, is not the same as the propellant fluid, or second fluid, used in the jack 22. In other words, there has no bypass in the conduits of the first fluid to supply the jack 22.
  • the device is used in a mode of descent of the piston 36 to compact the chromatographic bed 14 in the column 12.
  • the column 12 is previously filled with the material forming the bed 14.
  • the hydraulic fluid is then sent to the chamber 28 of the jack 22 in order to lower the piston 36 into the column 12 until the piston 36 comes into contact with the bed 14 and ensures its compaction.
  • the digital valve 48 and the control valve 50 are closed.
  • the device allows the piston 36 to be raised to allow the bed 14 to be emptied from the column 12.
  • the hydraulic fluid is sent to the chamber 30 of the jack 22 in order to reassemble the piston 36.
  • the valve TOR 48 and the control valve 50 are also closed.
  • the device is used for the separation of at least two compounds from a liquid to be chromatographed. The process includes the steps:
  • the separation of the compounds is accompanied by the regulation of the pressure exerted on the bed 14.
  • Al is the surface of the piston 36 in the column 12 and A2 is the surface of the piston 24 in the chamber 28.
  • equation 3 shows that PI can be kept constant at the value of Pcl by varying Ph. To do this, it is necessary to measure the hydraulic pressure Ph and the flow pressure at entry of column 12.
  • the use of a regulator 52 of the PI, PD, PID type allows the pressure on the bed 14 to be adjusted according to the steps:
  • the separation process can then be completed by the step of introducing the hydraulic liquid into the chamber 28 and the step of regulating the pressure in the chamber 28.
  • the flow pressure drops to zero.
  • the regulator 52 derives the hydraulic fluid in the bypass duct 42 by opening the TOR valve 48 and by opening the control valve 50 at a percentage controlled by the regulator 52.
  • the hydraulic fluid sent by the hydraulic source 44 does not enter the chamber 28 but is diverted into the bypass duct 42. It is then evacuated towards the hydraulic source 44. In this way, the pressure in the chamber 28 is reduced, generating less pressure from the piston 36 on the bed 14.
  • the adjustment of the pressure exerted by the piston 36 on the bed 14 makes it possible to adapt to the movements of the bed 14 when the latter inflates, for example.
  • the increase in the volume of the bed 14 would result in an increase in the mechanical pressure of the bed PI which would become greater than the set pressure Pcl.
  • the hydraulic fluid cannot exit from the upper chamber 28 of the cylinder 22, and an increase in the pressure PI would result in an increase in the hydraulic pressure. It is therefore necessary in this case to evacuate the hydraulic fluid from the chamber 28 in order to keep PI constant.
  • the digital valve 48 is open and the control valve 50 is open at a percentage controlled by the regulator 52, allowing the pressure PI to be kept constant and equal to Pcl.
  • the regulation of the pressure of the piston 36 on the bed 14 makes it possible to adapt to the operating conditions of the device. It provides all the efficiency of the bed 14 while protecting it.
  • the device described above is not limited to a single piston compacting the bed 14 but it is possible to envisage the action of two pistons on the bed 14.
  • the skilled person will able to use other types of cylinders such as pneumatic cylinders.
  • the chromatography device according to the invention is advantageously used in a method of separation by SMB, Simulated Moving Bed (US 2,985,589, US 3,291,726, US 3,268,605 and US 3,268,604 belonging to UOP, US 5,578,215 and US 5,578,216 belonging to IFP and NONASEP, EP 471,082 and EP 563,388 belonging to DAICEL) or in a process by NARICOL (US 6,136,198).
  • SMB Simulated Moving Bed
  • Simulated Moving Bed US 2,985,589, US 3,291,726, US 3,268,605 and US 3,268,604 belonging to UOP
  • US 5,578,215 and US 5,578,216 belonging to IFP and NONASEP EP 471,082 and EP 563,388 belonging to DAICEL
  • NARICOL US 6,136,198

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
EP02761925A 2001-04-10 2002-04-09 Schutzeinrichtung für das chromatographische bett in dynamischen axialkompressionschromatographiesäulen Withdrawn EP1379867A1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0104866A FR2823134B1 (fr) 2001-04-10 2001-04-10 Dispositif de protection du lit chromatographique dans les colonnes chromatographiques a compression axiale dynamique
FR0104866 2001-04-10
PCT/FR2002/001223 WO2002084275A1 (fr) 2001-04-10 2002-04-09 Dispositif de protection du lit chromatographique dans les colonnes chromatographique a compression axiale dynamique

Publications (1)

Publication Number Publication Date
EP1379867A1 true EP1379867A1 (de) 2004-01-14

Family

ID=8862156

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02761925A Withdrawn EP1379867A1 (de) 2001-04-10 2002-04-09 Schutzeinrichtung für das chromatographische bett in dynamischen axialkompressionschromatographiesäulen

Country Status (4)

Country Link
US (1) US7132053B2 (de)
EP (1) EP1379867A1 (de)
FR (1) FR2823134B1 (de)
WO (1) WO2002084275A1 (de)

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Also Published As

Publication number Publication date
FR2823134A1 (fr) 2002-10-11
FR2823134B1 (fr) 2003-09-19
US20040099604A1 (en) 2004-05-27
US7132053B2 (en) 2006-11-07
WO2002084275A1 (fr) 2002-10-24

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