FLUID PROCESSING DEVICE AND PROCESSING LIQUID RECOVERY METHOD

Abstract

A fluid processing system includes: a fluid processing section that performs a treatment of a sample while flowing fluid through a channel, the fluid after passage through the fluid processing section including gas and liquid; a gas-liquid separation section that is connected to an outlet side of the back pressure valve, that includes a gas-liquid separation pipe made of material letting the gas through and not letting the liquid through, and that discharges a gas phase in the fluid flowing through the gas-liquid separation pipe to an outside of the gas-liquid separation pipe; and a liquid phase collecting section that is provided on a downstream of the gas-liquid separation section and that recovers the liquid after passage through the gas-liquid separation section.

Claims

1-9. (canceled)

10. A super-critical fluid system for performing separation or extraction of a sample component by using super-critical fluid comprising: a fluid processing section which comprises a mobile phase delivery channel through which mixed fluid of carbon dioxide and modifier is delivered as a mobile phase and a back pressure valve that regulates a pressure in the mobile phase delivery channel so as to keep the mobile phase in a super-critical state in the mobile phase delivery channel, wherein the fluid which flows out from the fluid processing section is including carbon dioxide as a gas phase and modifier as a liquid phase; a gas-liquid separation section connected to an outlet of the back pressure valve at a downstream of the fluid processing section, the gas-liquid separation section comprises a gas-liquid separation pipe formed by material which allows gas through and does not allow liquid through, wherein the carbon dioxide included in the fluid which flows out from the outlet of the back pressure valve becomes a state of gas phase, the modifier included in the fluid which flows out from the outlet of the back pressure valve maintain a state of liquid phase, and the liquid phase is separated from the gas phase by discharging the gas phase in the fluid flowing through the gas-liquid separation pipe to an outside of the gas-liquid separation pipe through a wall face of the gas-liquid separation pipe; and a liquid phase collecting section provided on a downstream of the gas-liquid separation section and collects the liquid phase separated from the gas phase in the gas-liquid separation section.

11. The super-critical fluid system according to claim 10, wherein the gas-liquid separation section includes a pressurization section that maintains an inside of the gas-liquid separation pipe at a pressure higher than an atmospheric pressure.

12. The super-critical fluid system according to claim 11, wherein a channel segment having a smaller inside diameter than the gas-liquid separation pipe is provided as the pressurization section to a downstream end of the gas-liquid separation pipe or on a downstream of the downstream end of the gas-liquid separation pipe.

13. The super-critical fluid system according to claim 11, wherein a pressure regulating valve, that regulates a pressure in the gas-liquid separation pipe so that the pressure becomes a predetermined pressure higher than the atmospheric pressure, is provided as the pressurization section on a downstream of the gas-liquid separation pipe.

14. The super-critical fluid system according to claim 10, wherein the gas-liquid separation section includes a pressure reducing mechanism that reduces a pressure around the gas-liquid separation pipe to a pressure lower than a pressure in the gas-liquid separation pipe.

15. The super-critical fluid system according to claim 10, wherein the gas-liquid separation pipe is made of polytetrafluoroethylene.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0025] FIG. 1 is a channel structure diagram schematically showing an embodiment of a super-critical fluid chromatograph.

[0026] FIG. 2 is a structure diagram schematically showing an example of a structure of a gas-liquid separator.

[0027] FIG. 3 is a structure diagram schematically showing another example of the structure of the gas-liquid separator.

[0028] FIG. 4 is a structure diagram schematically showing yet another example of the structure of the gas-liquid separator.

EMBODIMENT OF THE INVENTION

[0029] An embodiment of a fluid processing system according to the present invention will be described below by using the drawings.

[0030] An embodiment of a super-critical fluid system which is one of the fluid processing systems is shown in FIG. 1.

[0031] The super-critical fluid system according to the embodiment includes a fluid processing section 1 for performing an analytical process of components while flowing fluid through a channel, a gas-liquid separation section 24, and a liquid phase collecting section 27. The fluid processing section 1 includes a mobile phase delivery channel 2, a sample injection section 14, an analytical column 16, a detector 20, and a back pressure valve 22. The sample injection section 14, the analytical column 16, and the detector 20 are provided on the mobile phase delivery channel 2 in this order from an upstream. The back pressure valve 22 is connected to a downstream end of the mobile phase delivery channel 2.

[0032] The gas-liquid separation section 24 is provided on a downstream of the back pressure valve 22 and the liquid phase collecting section 27 is provided on a downstream of the gas-liquid separation section 24. The liquid phase collecting section 27 includes a channel switching valve 28 connected to the downstream of the gas-liquid separation section 24 and a plurality of collecting containers 30a to 30d connected to respective ports of the channel switching valve 28. Although the four collecting containers 30a to 30d are shown in the embodiment, any number of collecting containers may be provided.

[0033] On an upstream of the mobile phase delivery channel 2, delivery pumps 8, 10 for respectively delivering carbon dioxide and modifier in liquid states and a mixer 12 for mixing the carbon dioxide and the modifier are provided. Carbon dioxide delivered from a carbon dioxide cylinder 4 by the delivery pump 8 and the modifier delivered from a modifier container 6 by the delivery pump 10 are mixed by the mixer 12 to become mixed fluid and flows through the mobile phase delivery channel 2 as a mobile phase.

[0034] The back pressure valve 22 is controlled so that a pressure in the mobile phase delivery channel 2 becomes a predetermined pressure (e.g., 10 MPa). In this way, carbon dioxide in the mobile phase flows in a super-critical state through the mobile phase delivery channel 2.

[0035] A sample to be analyzed is introduced into the mobile phase delivery channel 2 by the sample injection section 14. The analytical column 16 is connected to a downstream of the sample injection section 14 and the sample introduced into the mobile phase delivery channel 2 via the sample injection section 14 is separated into the components in the analytical column 16. The analytical column 16 is housed in a column oven 18 and a temperature of the analytical column 16 is kept constant. The detector 20 is connected to a downstream of the analytical column 16 and the sample components eluted from the analytical column 16 are consecutively introduced into the detector 20.

[0036] The back pressure valve 22 is connected to a downstream of the detector 20 and the gas-liquid separation section 24 is provided on an outlet side of the back pressure valve 22. The gas-liquid separation section 24 includes a gas-liquid separation pipe 26. The gas-liquid separation pipe 26 is a pipe formed by material which allows gas through and does not allow liquid through. An example of the material of the gas-liquid separation pipe is PTFE (polytetrafluoroethylene). The gas-liquid separation section 24 separates the fluid flowing out of the outlet of the back pressure valve 22 into the gas phase and the liquid phase by utilizing the gas-liquid separation pipe 26.

[0037] Carbon dioxide in the fluid flowing out of the outlet of the back pressure valve 22 is vaporized to be the gas phase due to rapid reduction in pressure. On the other hand, the modifier is in the liquid state before and after the back pressure valve 22. Almost entire quantities of the sample components eluted from the analytical column 16 are dissolved in the modifier which is the liquid phase. The gas-liquid separation section 24 is formed to discharge carbon dioxide, which is the gas phase in the fluid flowing through the gas-liquid separation pipe 26, to an outside of the gas-liquid separation pipe 26 and to lead only the liquid phase to the channel switching valve 28 provided on the downstream.

[0038] The channel switching valve 28 of the liquid phase collecting section 27 is a rotary switching valve, for example, and connects a channel from the gas-liquid separation section 24 to one of the collecting containers 30a to 30d. The channel switching valve 28 switches the channel in synchronization with a detection signal from the detector 20. and the liquid phases including the respective sample components separated in the analytical column 16 are collected in the separate collecting containers 30a to 30d.

[0039] In the super-critical fluid system according to the embodiment, the gas phase is discharged to the outside of the channel in the gas-liquid separation section 24, and therefore, only the liquid phases are dropped into the respective collecting containers 30a to 30d. Thus, vaporized carbon dioxide is not ejected from an outlet of the pipe communicating with the collecting containers 30a to 30d and the liquid phases are not scattered.

[0040] It is possible to enhance efficiency of the gas-liquid separation section 24 in separating the fluid into the gas and the liquid by providing a pressurization section for increasing a pressure in the gas-liquid separation pipe 26.

[0041] An example of the gas-liquid separation section 24 provided with the pressurization section is shown in FIG. 2.

[0042] In a structure in FIG. 2, a tubing 34 as the pressurization section is connected by a joint 32 to a downstream of the gas-liquid separation pipe 26. The tubing 34 has a smaller inside diameter than the gas-liquid separation pipe 26 and maintains an inside of the gas-liquid separation pipe 26 at a pressure (e.g., 3 MPa) higher than an atmospheric pressure. Because the pressure in the gas-liquid separation pipe 26 is maintained at the pressure higher than the atmospheric pressure, discharge of the gas phase in the fluid flowing through the gas-liquid separation pipe 26 to the outside of the gas-liquid separation pipe 26 is facilitated and the efficiency in separating the fluid flowing out of the outlet of the back pressure valve 22 into the gas and the liquid is enhanced.

[0043] Another example of the structure of the gas-liquid separation section 24 provided with the pressurization section is shown in FIG. 3.

[0044] In a structure in FIG. 3, a pressure sensor 36 is provided on a downstream of a gas-liquid separation pipe 26 and a pressure control valve 38 as the pressurization section is provided on a downstream of the pressure sensor 36. The pressure control valve 38 has a similar structure to the back pressure valve 22, for example. Operation of the pressure control valve 38 is controlled by a control section 40. The control section 40 controls the operation of the pressure control valve 38 based on a detection signal from the pressure sensor 36 so that a pressure in the gas-liquid separation pipe 26 becomes a pressure (e.g., 3 MPa) higher than an atmospheric pressure. The control section 40 may be used also as a control section for controlling operation of the back pressure valve 22, for example, as shown in FIG. 3.

[0045] With the structure in FIG. 3, as with the structure in FIG. 2, discharge of a gas phase in fluid flowing through the gas-liquid separation pipe 26 to an outside of the gas-liquid separation pipe 26 is facilitated, and efficiency in separating the fluid flowing out of an outlet of the back pressure valve 22 into gas and liquid is enhanced.

[0046] The pressurization section is not limited to those shown in FIGS. 2 and 3. For example, the pressure section may be any structure such as a structure including an orifice section having a smaller inside diameter than the gas-liquid separation pipe 26 and provided to a downstream end of the gas-liquid separation pipe 26 or on a downstream of the downstream end of the gas-liquid separation pipe 26, if the structure can maintain an inside of the gas-liquid separation pipe 26 at a pressure higher than an atmospheric pressure.

[0047] The efficiency of the gas-liquid separation section 24 in separating the fluid into the gas and the liquid is enhanced also by providing a pressure reducing section for reducing a pressure outside the gas-liquid separation pipe 26 instead of or in addition to the pressurization section.

[0048] An example of a structure of the gas-liquid separation section 24 provided with the pressure reducing section is shown in FIG. 4.

[0049] In a gas-liquid separation section 24 in this example, a gas-liquid separation pipe 26 is housed in a closed space 42. An inside of the closed space 42 is reduced in pressure to a pressure lower than an atmospheric pressure by a vacuum pump. Because the pressure in the gas-liquid separation pipe 26 is the atmospheric pressure or a pressure close to the atmospheric pressure, a pressure in the gas-liquid separation pipe 26 becomes relatively higher than the pressure around the gas-liquid separation pipe 26 when the pressure in the closed space 42 is reduced to the pressure lower than the atmospheric pressure. As a result, discharge of a gas phase in fluid flowing through the gas-liquid separation pipe 26 to an outside of the gas-liquid separation pipe 26 is facilitated, and efficiency in separating the fluid flowing out of an outlet of a back pressure valve 22 into gas and liquid is enhanced.

[0050] Although the pressure in the gas-liquid separation pipe 26 is the atmospheric pressure or the pressure close to the atmospheric pressure in the example in FIG. 4, the pressurization section shown in FIG. 2 or 3 may be used to increase the pressure in the gas-liquid separation pipe 26 to a pressure higher than the atmospheric pressure and the pressure reducing section shown in FIG. 4 may be also used to reduce the pressure outside the gas-liquid separation pipe 26 to a pressure lower than the atmospheric pressure. In this way, the discharge of the gas phase in the fluid flowing through the gas-liquid separation pipe 26 to the outside of the gas-liquid separation pipe 26 is further facilitated, and the efficiency in separating the fluid flowing out of the outlet of the back pressure valve 22 into the gas and the liquid is further enhanced.

[0051] Although the fluid flowing out of the outlet of the back pressure valve 22 is separated into the gas and the liquid by the gas-liquid separation section 24 and then only the liquid phases are introduced into the respective collecting containers 30a to 30d via the channel switching valve 28 in the super-critical fluid system described by using FIG. 1, the invention is not limited to this structure. Similar effects to those of the above-described embodiment can be obtained also by connecting a channel switching valve 28 to the downstream of the back pressure valve 22 without interposing the gas-liquid separation section 24 therebetween and providing the gas-liquid separation sections 24 between the channel switching valve 28 and the respective collecting containers 30a to 30d.

[0052] Although the super-critical fluid system described in the above embodiment is the super-critical fluid chromatograph for performing separation and analysis of the sample by using the super-critical fluid, the super-critical fluid system included in the embodiment is not limited to it. The system can be similarly applied to super-critical fluid extraction which is extraction of components included in a sample by use of super-critical fluid.

[0053] In addition to the above-described field of super-critical fluid, the invention can be similarly applied to the field of flow synthesis disclosed in Patent Document 3. In this case, as shown in FIG. 5, the above-described gas-liquid separation section 24 employing the gas-liquid separation pipe 26 can be used to remove a gas component (a gas phase) included in product liquid obtained in a final step of the flow synthesis section 46 (a fluid processing section) disclosed in Patent Document 3. A structure of the gas-liquid separation section 24 may be similar to those shown in FIGS. 2 to 4.

[0054] Although it is not shown in the figures, at least one column is provided on a channel through which liquid including raw material substances for synthesis flows in the flow synthesis section 46. A solid phase such as a catalyst which reacts with the row material substances is retained in the column. By passing the liquid including the raw material substances through the column, a reaction necessary for the synthesis occurs during the passage of the liquid. The liquid including a substance produced in the flow synthesis section 46 is introduced into the gas-liquid separation section 24 and an unnecessary gas component is removed in the gas-liquid separation section 24. The liquid phase after the removal of the unnecessary gas component in the gas-liquid separation section 24 is collected as processed liquid into a collecting container 48.

DESCRIPTION OF REFERENCE SIGNS

[0055] 1, 46: Fluid processing section [0056] 2: Mobile phase delivery channel [0057] 4: Carbon dioxide cylinder [0058] 6: Modifier container [0059] 8, 10: Delivery pump [0060] 12: Mixer [0061] 14: Sample injection section [0062] 16: Analytical column [0063] 18: Column oven [0064] 20: Detector [0065] 22: Back pressure valve [0066] 24: Gas-liquid separation section [0067] 26: Gas-liquid separation pipe [0068] 27: Liquid phase collecting section [0069] 28: Channel switching valve [0070] 30a to 30d, 48: Collecting container [0071] 32: Joint [0072] 34: Tubing [0073] 36: Pressure sensor [0074] 38: Pressure control valve [0075] 40: Control section [0076] 42: Closed space [0077] 44: Vacuum pump