A high-efficiency supercritical equipment

Abstract

The present invention discloses a high-efficiency supercritical fluid chromatography (SCF) system, relating to the technical field of chromatography. The system comprises a gas-liquid separator and a carbon dioxide filter connected by a pipeline. The gas-liquid separator is used to separate a gas-liquid mixture and convey the separated gas to the carbon dioxide filter. The carbon dioxide filter is used to filter the gas, and the filtered carbon dioxide is cooled by a refrigerator in a supercritical fluid chromatography system for reuse. The present invention can produce pure carbon dioxide in the component collection section of industrial-grade supercritical fluid chromatography, solving the problem of high carbon dioxide consumption and the inability to recycle carbon dioxide in industrial-grade supercritical fluid chromatography systems.

Description

Technical Field

[0001] The present invention relates to the technical field of chromatography, and in particular to a high-efficiency supercritical equipment. Background Art

[0002] Supercritical fluid chromatography uses a large amount of supercritical carbon dioxide instead of organic solvents as the mobile phase. Compared with ordinary liquid chromatography systems, it has the advantages of fast separation speed and environmental friendliness. Laboratory-grade supercritical fluid chromatographs have a small flow rate and a low carbon dioxide consumption, but industrial-grade supercritical fluid chromatography systems consume a lot of carbon dioxide. If discharged directly, the liquid carbon dioxide in the storage tank needs to be frequently replenished, and the supercritical fluid chromatography system cannot meet the conditions for long-term uninterrupted operation of industrial-grade equipment. Therefore, in industrial-grade supercritical fluid chromatography systems, it is often considered to collect the discharged gaseous carbon dioxide and then reuse it. The current technical difficulty lies in how to obtain pure carbon dioxide in the component collection part of industrial-grade supercritical fluid chromatography. Summary of the Invention

[0003] The purpose of the present invention is to provide a high-efficiency supercritical equipment to solve the problems existing in the above-mentioned prior art. It can obtain pure carbon dioxide in the industrial-grade supercritical fluid chromatography component collection part, and solve the problem that the industrial-grade supercritical fluid chromatography system consumes a lot of carbon dioxide and cannot be recycled.

[0004] To achieve the above object, the present invention provides the following solutions:

[0005] The present invention provides a high-efficiency supercritical equipment, comprising a gas-liquid separator and a carbon dioxide filter connected by a pipeline. The gas-liquid separator is used to separate a gas-liquid mixture into gas and liquid inside, gas passes through the upper end of the gas-liquid separator, and liquid passes through the lower end of the gas-liquid separator for collection. The separated gas is transported to the carbon dioxide filter, and the carbon dioxide after filtering is cooled by a refrigerator in a supercritical fluid chromatography system and then reused.

[0006] Optionally, a heater is further included, wherein the heater is serially connected to a heat exchanger, and the gas-liquid mixture enters the gas-liquid separator after being heated by the heat exchanger; a liquid heat exchange medium is provided in the heater, and the liquid heat exchange medium can be water. The heater provides hot water to the heat exchanger and the gas-liquid separator, and allows the hot water to circulate, and the temperature of the gas-liquid mixture after passing through the heat exchanger is changed by controlling the temperature of the hot water at the outlet of the heater. At the same time, the hot water is connected in series to control the temperature of the gas-liquid separator, and the environment of the gas-liquid mixture during gas-liquid separation is changed. Adjusting the temperature for different processes can achieve different gas-liquid separation effects. The heat exchanger heats the mixture of gaseous carbon dioxide and organic solvent with a lower temperature, and alleviates the mist state of the gas-liquid mixture before gas-liquid separation, thereby ensuring the separation effect after entering the gas-liquid separator.

[0007] Optionally, the gas-liquid separator is coated with a heating part, and the heater, heat exchanger and heating part are connected in series through pipelines.

[0008] Optionally, the carbon dioxide filter is filled with a tray filler, which can filter and condense the residual organic solvent and sample in the gas after passing through the gas-liquid separator again to obtain pure gaseous carbon dioxide for reuse in the supercritical fluid chromatography system.

[0009] Optionally, the carbon dioxide discharge port at the top of the carbon dioxide filter is connected to the refrigerator through a pipeline, and a temperature sensor is provided on the pipeline between the carbon dioxide discharge port and the refrigerator. The temperature sensor is electrically connected to the control end of the heater. The temperature sensor is used to detect the temperature of the gaseous carbon dioxide after gas-liquid separation, and feeds back the temperature detected here to the heater. By setting different temperature sensor temperatures to change the temperature of the hot water in the heater, a more suitable state in the gas-liquid separation process can be obtained.

[0010] Optionally, the liquid heat exchange medium is water.

[0011] Compared with the prior art, the present invention has achieved the following technical effects:

[0012] The present invention solves the problem of atomization of the gas-liquid mixture by changing the temperature of the gas-liquid mixture before the gas-liquid separator; achieves consistency between the temperature of the gas-liquid mixture and the temperature inside the gas-liquid separator by connecting hot water in series; further purifies gaseous carbon dioxide by using a carbon dioxide filter to ensure carbon dioxide purity; and automatically adjusts the ambient temperature of gas-liquid separation through feedback control of a temperature sensor to ensure the gas-liquid separation effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0014] Figure 1 It is a structural schematic diagram of the high-efficiency supercritical equipment of the present invention;

[0015] Among them, 1 is the heater, 101 is the hot water outlet of the heater, 102 is the hot water return port of the heater, 2 is the heat exchanger, 3 is the gas-liquid separator, 4 is the carbon dioxide filter, 5 is the temperature sensor, 6 is the gas-liquid mixture, and 7 is the refrigerator. DETAILED DESCRIPTION

[0016] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0017] The purpose of the present invention is to provide a high-efficiency supercritical equipment to solve the problems existing in the above-mentioned prior art. It can obtain pure carbon dioxide in the industrial-grade supercritical fluid chromatography component collection part, and solve the problem that the industrial-grade supercritical fluid chromatography system consumes a lot of carbon dioxide and cannot be recycled.

[0018] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0019] The present invention provides a high efficiency supercritical equipment, such as Figure 1 As shown, it includes a heater 1, a heat exchanger 2, a gas-liquid separator 3, a carbon dioxide filter 4, and a temperature sensor 5. The heater 1 includes a heater hot water outlet 101 and a heater hot water return port 102. The heater hot water outlet 101 is connected to the hot water inlet of the heat exchanger 2 by a pipeline. The hot water outlet of the heat exchanger 2 is connected to the hot water inlet of the gas-liquid separator 3 by a pipeline. The hot water outlet of the gas-liquid separator 3 is connected to the heater hot water return port 102 by a pipeline. The hot water from the heater 1 connects the heat exchanger 2 and the gas-liquid separator 3 in series through the pipeline to ensure that the temperature of the gas-liquid mixture is consistent with the temperature inside the gas-liquid separator.

[0020] The gas-liquid mixture 6 is connected to the inlet of the heat exchanger 2 via a pipeline. The outlet of the heat exchanger 2 is connected to the inlet of the gas-liquid separator 3 via a pipeline. The carbon dioxide discharge port at the top of the gas-liquid separator 3 is connected to the inlet of the carbon dioxide filter 4 via a pipeline. The carbon dioxide discharge port at the top of the carbon dioxide filter 4 is connected to the refrigerator 7 via a pipeline for recycling. A temperature sensor 5 is set in the middle of this section of the pipeline to measure the temperature of the carbon dioxide after gas-liquid separation. The carbon dioxide gas temperature detected by the temperature sensor 5 can provide real-time feedback on the gas-liquid separation effect and is fed back to the heater 1 via a signal to automatically control the hot water temperature of the heater 1 to ensure good gas-liquid separation effect. During the component collection stage of the supercritical fluid chromatography system, the supercritical carbon dioxide is depressurized and becomes gaseous. At this time, the mobile phase becomes a low-temperature gas-liquid mixture composed of gaseous carbon dioxide and a small amount of organic solvent, which exists in the form of a mist aerosol in the pipeline.

[0021] The present invention heats the gas-liquid mixture 6 through the heat exchanger 2 before the gas-liquid mixture enters the gas-liquid separator 3 to alleviate the state of the mist aerosol, and at this time the gas-liquid mixture 6 is easier to separate into gas and liquid. Gas-liquid separation is performed after entering the gas-liquid separator 3, and the discharged carbon dioxide gas will be mixed with trace amounts of organic solvents or samples. Through the carbon dioxide filter 4 connected at the back, when passing through the tower plate filler in the filter, trace amounts of organic solvents or samples will gradually condense to form small droplets, flow along the inner wall of the carbon dioxide filter 4 to the bottom, and the liquid will be temporarily stored at the bottom of the carbon dioxide filter 4. The valve at the bottom of the carbon dioxide filter 4 is controlled by software to be discharged regularly. At this time, the gaseous carbon dioxide discharged from the top of the carbon dioxide filter 4 is purer and can be cooled by the refrigerator in the supercritical fluid chromatography system and reused.

[0022] In the description of the present invention, it should be noted that the terms "center," "top," "bottom," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are intended solely to facilitate and simplify the description of the present invention. They do not indicate or imply that the devices or components referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limitations on the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0023] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only intended to help understand the method and core concept of the present invention. At the same time, those skilled in the art will find that the specific implementation methods and application scopes may vary based on the concept of the present invention. In summary, the contents of this specification should not be construed as limiting the present invention.

Claims

1. A high-efficiency supercritical equipment, characterized by: The invention comprises a gas-liquid separator and a carbon dioxide filter connected by a pipeline, wherein the gas-liquid separator is used to separate a gas-liquid mixture and transport the separated gas to the carbon dioxide filter, and the carbon dioxide filter is used to filter the gas and reuse the filtered carbon dioxide after cooling by a refrigerator in a supercritical fluid chromatography system; the invention also comprises a heater, wherein the heater is serially connected to a heat exchanger, and the gas-liquid mixture enters the gas-liquid separator after being heated by the heat exchanger; a liquid heat exchange medium is arranged in the heater; the gas-liquid separator is coated with a heating part, and the heater, heat exchanger and heating part are serially connected by a pipeline; hot water is connected in series to ensure that the temperature of the gas-liquid mixture is consistent with the temperature inside the gas-liquid separator; the carbon dioxide filter is filled with a tower plate filler, and the tower plate filler can filter and condense the organic solvent and sample remaining in the gas after passing through the gas-liquid separator again to obtain pure gaseous carbon dioxide.

2. The high-efficiency supercritical equipment according to claim 1, characterized in that: The carbon dioxide discharge port at the top of the carbon dioxide filter is connected to the refrigerator through a pipeline. A temperature sensor is provided at the pipeline between the carbon dioxide discharge port and the refrigerator. The temperature sensor is electrically connected to the control end of the heating machine.

3. The high-efficiency supercritical equipment according to claim 1, characterized in that: The liquid heat exchange medium is water.

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