Gas-liquid separator for a chromatography system

Abstract

The present invention relates to a gas-liquid separator for a chromatography system, comprising: a) a separating region having an inlet nozzle, a baffle unit and a gas distribution unit; (b) a dividing region having a liquid outlet; and (c) a gas discharge region having a gas outlet; wherein the separating region is connected to the dividing region by a separating opening and the distance of the inlet nozzle from the baffle unit is greater than the smallest longitudinal extension of the separating opening and the inlet nozzle is configured such that a gas-liquid stream directed through the inlet nozzle can act on the baffle unit. The present invention further relates to a chromatography system comprising a separator according to the invention and to a chromatography method wherein the separator is used.

Claims

1. A gas-liquid separator for a chromatography system comprising: a) a separating region having an inlet nozzle, a baffle unit, and a gas distribution unit; (b) a dividing region having a liquid outlet; and (c) a gas discharge region having a gas outlet; wherein: the separating region is connected to the dividing region by a separating opening and a distance of the inlet nozzle from the baffle unit is greater than a smallest longitudinal extension of the separating opening and the inlet nozzle is configured such that a gas-liquid stream directed through the inlet nozzle can act on the baffle unit, the separating region does not have a circular cross-sectional area in a region of the inlet nozzle, and the gas-liquid separator is operable with a stream direction of the gas in the separating region which is parallel to a stream direction of the liquid, the separating opening is configured such that a stream velocity of the gas in the dividing region is reduced, and the baffle unit is not bent and functions as a baffle plate.

2. The gas-liquid separator according to claim 1, wherein the separating opening has two, three, four, or more partial separating openings, by arrangement of which a reduction in the stream velocity of the gas is effectible.

3. The gas-liquid separator according to claim 1, wherein the gas-liquid separator has installations in the dividing region for reducing the gas stream.

4. The gas-liquid separator according to claim 1, wherein a diverting unit is provided in the separating region, by which an aerosol stream can act on a second baffle unit.

5. A method of separating a gas-liquid mixture comprising using a gas-liquid separator according to claim 1.

6. The gas-liquid separator according to claim 1, wherein the separating region comprises at least three side walls which, together with an upper end, define a space which is connected to the dividing region by the separating opening.

7. The gas-liquid separator according to claim 1, wherein said baffle plate forms a wall of the separating region and constitutes a side wall of the gas distribution unit.

8. The gas-liquid separator according to claim 1, wherein the stream direction of the gas and the stream direction of the liquid are parallel in a lower region of the separating region.

9. The gas-liquid separator according to claim 8, wherein the stream direction of the gas and the stream direction of the liquid are parallel in a lower third of the separating region.

10. The gas-liquid separator according to claim 1, wherein the separating region comprises at least two side walls defining, together with an upper end and a gas acceleration unit, a space forming the gas distribution unit, wherein one of the side walls, the gas acceleration unit, or the upper end is formed as a baffle unit, wherein said space is connected to the dividing region by the separating opening, and wherein a distance between two opposite side walls is greater than half a distance of the inlet nozzle from the baffle unit.

11. The gas-liquid separator according to claim 10, wherein the separating region comprises at least three side walls defining, together with the upper end and the gas acceleration unit, a space forming the gas distribution unit, wherein one of the side walls, the gas acceleration unit, or the upper end is formed as a baffle unit, wherein said space is connected to the dividing region by the separating opening, and wherein the distance between two opposite side walls is greater than half a distance of the inlet nozzle from the baffle unit.

12. A chromatography system comprising at least one gas-liquid separator according to claim 1.

13. A method of separating a gas-liquid mixture comprising using a chromatography system according to claim 12.

14. The gas-liquid separator according to claim 1, wherein a ratio of an entry surface of the inlet nozzle provided in the separating region to a volume of the separating region is in the range from 4:1 mm.sup.2/mL to 1:50 mm.sup.2/mL.

15. The gas-liquid separator according to claim 14, wherein the ratio of the entry surface of the inlet nozzle provided in the separating region to the volume of the separating region is in the range from 1:1 mm.sup.2/mL to 1:20 mm.sup.2/mL.

16. The gas-liquid separator according to claim 15, wherein the ratio of the entry surface of the inlet nozzle provided in the separating region to the volume of the separating region is in the range from 2:3 mm.sup.2/mL to 1:5 mm.sup.2/mL.

17. The gas-liquid separator according to claim 1, wherein a ratio of an outlet surface of the separating opening to a volume of the gas-liquid separator is in the range from 0.05 mm.sup.2/mL to 6 mm.sup.2/mL.

18. The gas-liquid separator according to claim 17, wherein the ratio of the outlet surface of the separating opening to the volume of the gas-liquid separator is in the range from 0.3 mm.sup.2/mL to 3 mm.sup.2/mL.

19. The gas-liquid separator according to claim 18, wherein the ratio of the outlet surface of the separating opening to the volume of the gas-liquid separator is in the range from 0.5 mm.sup.2/mL to 2.0 mm.sup.2/mL.

20. The gas-liquid separator according to claim 1, wherein the inlet nozzle is configured such that a gas-liquid stream directed through the inlet nozzle can act on the baffle unit.

21. The gas-liquid separator according to claim 20, wherein an angle at which a gas-liquid stream directed through the inlet nozzle can act on the baffle unit is in the range from 50° to 130°.

22. The gas-liquid separator according to claim 21, wherein an angle at which a gas-liquid stream directed through the inlet nozzle can act on the baffle unit is in the range from 70° to 110°.

23. The gas-liquid separator according to claim 1, wherein the baffle unit has a surface region with a surface energy in the range from 15 mN/m to 120 mN/m.

24. The gas-liquid separator according to claim 23, wherein the surface region has a surface energy in the range from 20 mN/m to 80 mN/m.

25. The gas-liquid separator according to claim 24, wherein at least 80% of the surface of the baffle unit has a surface energy in the range from 20 mN/m to 80 mN/m.

26. The gas-liquid separator according to claim 25, wherein at least 90% of the surface of the baffle unit has a surface energy in the range from 20 mN/m to 80 mN/m.

27. The gas-liquid separator according to claim 23, wherein the surface region has a surface energy in the range from 22 mN/m to 60 mN/m.

28. The gas-liquid separator according to claim 27, wherein at least 80% of the surface of the baffle unit has a surface energy in the range from 22 mN/m to 60 mN/m.

29. The gas-liquid separator according to claim 28, wherein at least 90% of the surface of the baffle unit has a surface energy in the range from 22 mN/m to 60 mN/m.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) In the following, preferred embodiments of the present invention are described by way of example using drawing figures, without a limitation of the invention being thereby intended. Therein:

(2) FIG. 1 shows a schematic longitudinal sectional view of a gas-liquid separator according to the invention,

(3) FIG. 2 shows a schematic cross-sectional view of a gas-liquid separator according to the invention,

(4) FIG. 3 shows a schematic view of a gas-liquid separator according to the invention,

(5) FIG. 4 shows a schematic longitudinal representation of a further embodiment of a gas-liquid separator according to the invention,

(6) FIG. 5 shows a schematic longitudinal sectional view of a further embodiment of a gas-liquid separator according to the invention,

(7) FIG. 6 shows a schematic longitudinal sectional view of a further embodiment of a gas-liquid separator according to the invention

(8) FIG. 7 shows a schematic longitudinal sectional view of a further embodiment of a gas-liquid separator according to the invention,

(9) FIG. 8 shows a schematic longitudinal sectional view of the embodiment of a gas-liquid separator according to the invention as shown in FIG. 7, wherein the sectional plane is rotated by 90° with respect to the sectional plane shown in FIG. 7,

(10) FIG. 9 shows a schematic longitudinal sectional view of a further embodiment of a gas-liquid separator according to the invention,

(11) FIG. 10 shows a schematic view of a chromatography system with a gas-liquid separator according to the invention.

DETAILED DESCRIPTION OF THE DRAWINGS

(12) FIG. 1 describes a gas-liquid separator 10 according to the invention in a longitudinal sectional view.

(13) The gas-liquid separator 10 comprises a separating region 12 having an inlet nozzle 14, a baffle unit 16 and a gas distribution unit 18. The gas distribution unit 18 is formed by the baffle unit 16 of a gas acceleration plate 20, which is configured herein as a baffle plate, as well as two further side walls, which are not shown in the longitudinal section. In particular, the wedge-shaped shape of the separating region 12 is shown, through which a gas is accelerated from the region of the inlet nozzle 14 to the separating opening 22.

(14) The baffle unit 16 configured herein as a baffle plate can have a structured or smooth surface. The gas acceleration plate 20 may be flat or slightly concavely curved from the inlet nozzle 14 in the direction of the separating opening 22 so as to reduce the apparent decrease in the distance between the baffle plate 16 and the gas acceleration plate 20. The separating region 12 is capped by an upper end 24.

(15) The gas-liquid separator 10 comprises a dividing region 26 having a liquid outlet 28, wherein the dividing region 26 is connected to the separating region 12 by the separating opening 22, so that the separating region 12 is in fluid contact with the dividing region 26.

(16) The baffle unit 16 configured herein as a baffle plate forms a side wall of the dividing region 26. The bottom of the gas-liquid separator 10 is formed by the lower end of the dividing region 26. This bottom can be configured such that the liquid outlet 28 is provided at the lowest point of the bottom.

(17) A side wall 32 of the gas discharge region 30 and the two side walls not shown in the longitudinal section together with an opening 34 provided between the gas discharge region 30 and the dividing region 26 and the separating opening 22 form the further boundaries of the dividing region.

(18) In the dividing region 26, the gas phase is divided from the liquid phase, wherein the gas is preferably accelerated by the gas distribution unit 18 in the direction of the separating opening 22, so that the liquid is transferred in the direction of the bottom of the dividing region 26.

(19) The gas phase is led through the opening 34, which is provided between the gas discharge region 30 and the dividing region 26, into the gas discharge region 30. The gas discharge region 30 is configured herein in such a way that the gas is accelerated in the direction of the gas outlet 35, which is provided in the gas discharge region 30.

(20) In this case, the rear wall of the gas acceleration plate 20 described above together with the side wall 32 projecting into the dividing region forms a corresponding wedge shape, wherein one edge of the gas acceleration plate 20 is connected to the side wall 32.

(21) FIG. 2 shows a schematic cross-sectional view of a gas-liquid separator 10 according to the invention, wherein identical reference signs describe identical parts.

(22) In particular, the side walls 36, 38 of the gas-liquid separator 10, which were not shown before, are visible. Furthermore, the aerosol supply line 40 and the gas discharge line 42 are shown.

(23) Furthermore, it can be seen that in this configuration the baffle unit 16, which is configured as an impact plate, has a groove-shaped surface structure.

(24) FIG. 3 shows a schematic view of a gas-liquid separator 10 according to the invention, wherein identical reference signs describe identical parts. In particular, the preferred configuration of the lower end 44 of the dividing region 26 and the upper end 24 of separating region 12 is evident, each of which has an arc-shaped design.

(25) FIG. 4 describes a gas-liquid separator 50 according to the invention in a longitudinal sectional view.

(26) The gas-liquid separator 50 comprises a separating region 52 having an inlet nozzle 54, a baffle unit 56 and a gas distribution unit 58. The gas distribution unit 58 is formed by a gas acceleration unit 60, two side walls 62a, 62b, and another bottom wall and a top wall, which are not shown in the longitudinal section. In particular, the wedge-shaped shape of the separating region 52 is shown, through which a gas is accelerated from the region of the inlet nozzle 54 to the separating opening 64.

(27) In the present embodiment, the separating region 52 is divided into two subregions 52a, 52b, each of which is connected to dividing region 66 via its own partial separating openings 64a and 64b.

(28) In the present embodiment, the baffle unit 56 is formed in the region of the gas acceleration unit 60, which at this point connects the two subregions 60a, 60b of the gas acceleration unit 60 in an arc and partially divides the subregions 52a, 52b of the separating region 52. The inlet nozzle 54 directs the gas-liquid mixture onto the baffle unit 56. This creates a gas stream that runs parallel to the stream direction of the liquid in the separating region 52. Herein, the gas acceleration unit 60 has two subregions 60a, 60b which lead from the inlet nozzle 54 in the direction of the separating opening 64 to a reduction of the distance between the gas acceleration unit 60 and the respective side wall 62a, 62b, wherein the subregions 60a, 60b of the gas acceleration unit 60 can be flat or slightly concavely curved. The separating region 52 is capped by an upper end 68.

(29) The gas-liquid separator 50 comprises a dividing region 66 having a liquid outlet 70, wherein the dividing region 66 is connected to the separating region 52 by the separating opening 64 and the two partial separating openings 64a and 64b respectively, so that the two subregions 52a, 52b of the separating region 52 are in fluid contact with the dividing region 66.

(30) The bottom of the gas-liquid separator 50 is formed by the lower end of the dividing region 66. This bottom can be configured such that the liquid outlet 70 is provided at the lowest point of the bottom.

(31) The gas discharge region 72 is formed by the gas acceleration unit 60 and the two walls not shown in the longitudinal section together with an opening 74 provided between the gas discharge region 72 and the dividing region 66.

(32) In the dividing region 66, the gas phase is divided from the liquid phase, wherein the gas is preferably accelerated by the gas distribution unit 58 in the direction of the separating opening 64, so that the liquid is transferred in the direction of the bottom of the dividing region 66. In the present embodiment, the two partial gas streams are led through the partial separating openings 52a, 52b into the dividing region 66 and are directed against each other so that their velocity in the dividing region is minimized. Through this configuration, the amount of liquid entrained in the gas stream can be greatly reduced.

(33) The gas phase is led through the opening 74, which is provided between the gas discharge region 72 and the dividing region 66, into the gas discharge region 72. The gas discharge region 72 is configured herein in such a way that the gas is accelerated in the direction of the gas outlet 76, which is provided in the gas discharge region 72.

(34) In this case, the rear side of the gas acceleration unit 60 described above forms a corresponding shape that narrows upwards.

(35) The embodiment shown in FIG. 4 can be very easily manufactured by milling from a plastic block. In this case, the rear wall not shown in FIG. 4 can be manufactured by leaving the material intact, wherein the volumes of the previously described regions and subregions can be maintained by corresponding milling depths or depths of material removal. The upper side can be provided by a plate, for example a glass plate, which is pressed from above against the milled plastic block. Pressing can, for example, be achieved by means of a screw connection. The corresponding bores are indicated by the reference sign 78. The plate forming the top is preferably fixed by a recess provided in steps over the regions and subregions set out, which can be regarded as a groove. This step-shaped recess is indicated herein by the reference sign 79.

(36) FIG. 5 describes a gas-liquid separator 80 according to the invention in a longitudinal sectional view. The conceptual construction of the gas-liquid separator 80 shown in FIG. 5 corresponds to the gas-liquid separator 50 shown in FIG. 4, wherein identical or similar components have the same reference signs. The gas-liquid separator 80 comprises a separating region 52 having an inlet nozzle 54, a baffle unit 56 and a gas distribution unit 82.

(37) The gas distribution unit 82 is formed by a gas acceleration unit 84, two side walls 62a, 62b, and another bottom wall and a top wall, which are not shown in the longitudinal section.

(38) The substantial difference is in particular that the gas acceleration unit 84 divides itself sharply into two subregions 88a and 88b, in contrast to the gas acceleration unit 60 of the configuration shown in FIG. 4, which is formed to be curved in the impact region. In this case, the nozzle is directed onto the impact region 56, which can be formed to be relatively flat so that the joint between the two subregions 84a and 84b is flattened.

(39) FIG. 6 describes a gas-liquid separator 90 according to the invention in a longitudinal sectional view. The conceptual construction of the gas-liquid separator 90 shown in FIG. 6 corresponds to the gas-liquid separator 80 shown in FIG. 5, wherein identical or similar components have the same reference signs. The gas-liquid separator 90 comprises a separating region 52 with two inlet nozzles 94a, 94b, a baffle unit 56 and a gas distribution unit 82.

(40) The substantial difference is in particular that the two inlet nozzles 94a, 94b direct the aerosol onto the gas distribution unit 82 from two sides or onto the two subregions 82a, 82b of the gas distribution unit 82. It is apparent to the person skilled in the art that the gas distribution unit 82 could be separated at the upper end 68 by a dividing wall into two actually divided separating regions without there being any substantial changes in the stream in the dividing region.

(41) FIG. 7 describes a gas-liquid separator 100 according to the invention in a longitudinal sectional view. The conceptual construction of the gas-liquid separator 100 shown in FIG. 7 corresponds to the gas-liquid separator 50 shown in FIG. 4, wherein identical or similar components have the same reference signs. The gas-liquid separator 100 comprises a separating region 52 having an inlet nozzle 102 and a gas distribution unit 58. In its present form, the baffle unit is formed by the top wall, which is not shown in FIG. 7.

(42) The substantial difference is in particular that the baffle unit is formed by the top wall which is not shown, wherein the baffle unit is first directed through the inlet nozzle 102 into the gas-liquid separator 100 onto the top wall. The diverting unit 104 directs the gas stream to the upper end 106, which has an inner curvature 108 in the present embodiment. The diverting unit 104 is formed by a recess from the gas acceleration unit 110, which at this point connects the two subregions 110a, 110b of the gas acceleration unit 110 in an arc and partially divides the subregions 52a, 52b of the separating region 52.

(43) Accordingly, the upper end 106, in particular the region of the inner curvature 108, can be regarded as a second baffle unit since part of the aerosol undergoes further impact separation. The inner curvature 108 stabilizes the gas stream, so that the aerosol or gas stream is directed to the two subregions 52a and 52b of the gas distribution unit.

(44) FIG. 8 shows a longitudinal view of the gas-liquid separator 100 described in FIG. 7, wherein a sectional plane is shown which is perpendicular to the view shown in FIG. 7. The plane shown shows a section through the tip of the inner curvature 108 and the liquid outlet 70. In particular, the top wall 112 and the bottom wall 114 are shown. The line 116 represents the bottom region of the diverting unit 104 and the line 118 represents the tip of the inner curvature 108. The dashed lines 120, 122 indicate the material milled slots which form the diverting unit 104, while the dashed line 124 indicates the upper region of the gas discharge region 72, wherein, at this point, the gas is collected and transferred to the gas outlet 76.

(45) FIG. 9 describes a gas-liquid separator 130 according to the invention in a longitudinal sectional view. The conceptual construction of the gas-liquid separator 130 shown in FIG. 9 corresponds to the gas-liquid separator 50 shown in FIG. 4, wherein identical or similar components have the same reference signs. The gas-liquid separator 130 comprises a separating region 52 with two inlet nozzles 134a, 134b, two baffle units 136a, 136b and a gas distribution unit 52.

(46) The substantial difference is in particular that the two inlet nozzles 134a, 134b direct the aerosol onto the opposite sides of the respective side walls 62a, 62b, which are formed at the respective points as baffle units 136a, 136b, wherein the jet of the inlet nozzles 134a is directed onto the baffle unit 136a, which can be regarded as part of the side wall 62b. In this case, the two inlet nozzles 134a, 134b can be easily slightly moved in a horizontal or vertical direction.

(47) The embodiments shown in FIGS. 5 to 9 may, as previously shown for FIG. 4, be produced by milling from a plastic block, with the top being provided by a plate, such as a glass plate, which is pressed from above against the milled plastic block. Furthermore, all embodiments can be provided by casting or similar methods.

(48) FIG. 10 shows a schematic view of a chromatography system 200 with a gas-liquid separator 230 according to the invention, which is suitable for supercritical liquid chromatography.

(49) Such a system is described by way of example using supercritical CO.sub.2, wherein methanol is shown as an exemplary solvent. Of course, systems in which other solvents, preferably organic solvents, or other supercritical fluids are used, are similarly constructed.

(50) As shown in FIG. 9, the respective fluids are stored in storage tanks, in particular the gas which is further used in a supercritical state is provided in a storage tank 202 and the solvent in a storage tank 204, each of which can be conveyed from the storage tanks 202, 204 by a pump 206, 208 to become the further components of the system. In the System 200 described here, a preparation stage 210, 212 is preferably provided in each fluid supply line, via which the liquids can be tempered. It is further possible to level the pressure fluctuations indicated by the pumps. Accordingly, this preparation stage can, for example, be formed as a heat exchanger or pump. An addition unit 214 may preferably be provided in the solvent line, for example an injector via which a mixture to be separated is introduced into the system 200 before the CO.sub.2 and the solvent are fed into a mixer 216 and from this into a chromatography column 218.

(51) In this system 200, two analysis units are connected downstream of the chromatography column 218, wherein a sample discharge unit 220 is connected to a mass spectrometer 222 for this purpose and a UV detector 224 is provided downstream of the sample discharge unit. The back-pressure regulator 226 provided in the line maintains the respective pressure necessary for the fluid to remain in a supercritical state. After the back-pressure regulator 226, a heat exchanger 228 is provided which prevents the aerosol from freezing during the expansion process. Subsequently, the aerosol is introduced into a 230 gas-liquid separator according to the invention, wherein the gas of the system is discharged via outlet 232.

(52) The liquid is introduced into a fraction collector 234 and fractionated in the same. The solvent contained in the fractionated samples can be removed from the samples.

(53) The features of the invention revealed in the above description, as well as the claims, figures and examples of execution, may be essential both individually and in any combination for the realization of the invention in its embodiments.