JP2001038102A - Supercritical fluid extraction device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To repeatedly extract without discharging fluid to the outside until the extraction is completed by arranging switching valves respectively on an inlet pipe line of an extraction vessel and an outlet pipe line of an absorption vessel, connecting the pipe lines to each other with a pipe line provided with a circulation pump and switching respective switching valves. SOLUTION: A sample material is filled in the extraction vessel 3, an adsorbent is filled in the adsorption vessel 5 and carbon dioxide is supplied as the fluid form a fluid bomb 1. A supercritical state is formed by controlling to a prescribed pressure and temp. with a pressure pump 2, a pressure controller 6 and a temp. controller 11. After that, a circulation passage is formed by respectively switching plural switching valves 8, 9 and the fluid is circulated by the circulation pump 10. As a result, an extracting component in the sample material is dissolved in the circulating fluid and absorbed on the adsorbent while the extracting state is monitored by a detector 4. By repeating the extraction in this way, the extraction work of the fluid is improved.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a supercritical fluid extraction device using a supercritical fluid.

[0002]

2. Description of the Related Art An extraction method using a fluid in a supercritical state is safer than an extraction method using an organic solvent, and generally can be extracted under a temperature condition of about 40 ° C. to 80 ° C. Recently, it has attracted attention as a stable extraction method suitable for heat-unstable extraction substances.

FIG. 2 is a schematic diagram showing the configuration of a conventional supercritical fluid extraction apparatus employing, for example, carbon dioxide (CO ₂ ) as a fluid.
The extraction container 3, the detector 4, the pressure control device 6, and the collection container 7 are sequentially connected by piping.

In this apparatus, the fluid flowing through the extraction vessel 3 is subjected to a critical pressure (for example, dioxide) by a pressure pump 2 for increasing the pressure of the fluid at the fluid inlet side and a pressure control device 6 for adjusting the back pressure at the fluid outlet side. In addition to controlling the pressure to 73 atm or more in the case of carbon and controlling the temperature to be equal to or higher than the critical temperature (about 31 ° C. in the case of the same carbon dioxide) by the temperature control device 11 of the thermostatic bath type, the carbon dioxide is supercritical fluid ( (Hereinafter, simply referred to as a fluid), a desired component is extracted from the sample substance in the extraction container 3, and monitoring is performed by the detector 4. Next, the same fluid in which the extract is dissolved is led to the pressure control device 6, where the fluid is relieved and reduced to a predetermined pressure. Since the pressure at the outlet side of the pressure control device 6 is lower than that at the inlet side, the fluid returns to the original carbon dioxide, and the extracted components dissolved in the fluid are separated and separated, and collected in the collection container 7. You. In this case, if necessary, in order to increase the recovery efficiency of the extracted component, a method of providing an adsorption container 5 between the detector 4 and the pressure control device 6 and adsorbing a part or all of the extracted component may be employed. Adopted.

[0005]

As described above, the conventional supercritical fluid extraction device has a structure in which a part of the fluid is continuously released from the pressure control device 6, and the carbon dioxide is always newly supplied from the fluid cylinder 1. It was a method to keep sending. In other words, there is a problem that a large amount of fluid has to be used because the system is always in circulation. Further, since the fluid and the extracted components are continuously released from the pressure control device 6, there is a problem that the process environment is not always good.

The present invention has been made in order to solve the above-mentioned problems. A switching valve is provided at each of the inlet pipe of the extraction vessel and the outlet pipe of the adsorption vessel, and the switching valves are connected to each other by a pipe. At the same time, a circulation pump is provided in the middle of the pipe, and by switching the switching valve, a circulation system from the adsorption vessel to the extraction vessel is formed, and a predetermined amount of fluid is discharged to the outside until the extraction is completed. It is an object of the present invention to provide a supercritical fluid extraction device capable of repeatedly performing extraction through an extraction container without using the same.

[0007]

Means for Solving the Problems In order to achieve the above object, the present invention is provided with the following means for solving the problems.

That is, the supercritical fluid extraction device of the present invention is a supercritical fluid extraction device for extracting a desired component from a predetermined sample substance in a supercritical state of a predetermined fluid, comprising a pressure pump, an extraction vessel , A detector, an adsorption vessel, and a pressure control device are sequentially connected by a main pipe, and a switching valve is provided in each of an inlet pipe of the extraction vessel and an outlet pipe of the adsorption vessel, and a pipe is provided between these switching valves. And a circulation pump is provided in the middle of the pipe, and the switching valve is switched to form a circulation path from the adsorption vessel to the extraction vessel.

Therefore, with this configuration, the extraction can be repeatedly performed through the extraction container without discharging a predetermined amount of fluid to the outside through the circulation system until the extraction is completed. As a result, the amount of fluid used can be reduced, and extraction can be performed efficiently in a short time.

[0010]

Next, an embodiment of the present invention will be described in detail with reference to FIG.

That is, FIG. 1 is a flow chart showing a configuration of a supercritical fluid extracting apparatus according to an embodiment of the present invention. As shown in the drawing, this supercritical fluid extraction apparatus includes a fluid cylinder 1 filled with, for example, carbon dioxide (CO ₂ ), a pressurizing pump 2 for increasing the fluid pressure, and a first pump for storing a sample substance.
Extraction vessel 3, fluid inlet side first switching valve 8, detector 4 for monitoring the extraction level, adsorption vessel 5 for adsorbing the extracted components, fluid outlet side second switching valve 9, and relieving the fluid to the outside. Pressure control device 6 for controlling pressure (back pressure),
A collection vessel 7 for collecting the extracted components and a circulation pump 10 for circulating the fluid are sequentially connected by piping to form a main system passage and a circulation system described later.

The main route is a fluid cylinder 1, a pressure pump 2,
First switching valve 8, extraction container 3, detector 4, adsorption container 5, second switching valve 9, pressure control device 6, recovery container 7
It is composed of In this main path, a circulating system in which the first and second switching valves 8 and 9 are connected to each other by a pipe in a reverse direction, and a circulation pump 10 acting in a reverse flow direction is provided in the middle of the pipe. Roads are provided.

Therefore, in this configuration, the first and second
By switching the switching valves 8 and 9 from the main system path side to the circulation system path side, the extraction vessel 3, the detector 4, and the like between the first switching valve 8 and the second switching valve 9 of the main system path are switched. By switching the adsorption vessel 5 to a circulation path via the circulation pump 10, a predetermined fluid can always be circulated as indicated by the imaginary line of the arrow. Further, the temperature of each device and the piping section of the circulation system is controlled to a predetermined temperature (40 to 80 ° C.) by the temperature control device 11 of a constant temperature bath type which controls the temperature of the entire system, and the inside of the circulation system is controlled. The flowing fluid is controlled to a supercritical fluid state.

First, first, the extraction container 3 is filled with a sample substance, and the adsorption container 5 is filled with an adsorbent (for example, silica gel).
Begins to flow carbon dioxide as a fluid from. After the air in all the systems including the circulation system is replaced with carbon dioxide, the pressure and temperature are adjusted to a predetermined pressure and temperature by the pressurizing pump 2, the pressure control device 6, and the temperature control device 11, thereby setting the supercritical state. Form. Next, after the above-mentioned circulation system path is formed by switching the first and second switching valves 8 and 9, the fluid in the supercritical state is circulated by the circulation pump 10 as indicated by the imaginary line of the arrow. Then, a part of the extracted components in the sample substance in the extraction container 3 dissolves in the circulating fluid, and is adsorbed on the adsorbent in the adsorption container 5 while the extraction state is monitored by the detector 4. Is done.

[0015] Then, as described above, the extracted component is adsorbed on the adsorption vessel 5.
As it is adsorbed by the adsorbent inside, the extraction components in the fluid decrease, and the extraction power of the fluid increases. Then, the fluid having the increased extraction force is again introduced into the extraction container 3 via the circulation pump 10 and extraction is performed. This repetition is performed continuously, and the effect of extracting the extracted components of the fluid is greatly improved. On the other hand, the extracted component adsorbed on the adsorbent is subjected to the first and second switching valves 8 and
After the circulation path is cut off by the switching of 9 to return to the state of the original main path only, elution is performed by controlling the temperature and pressure under elution conditions and finally collected in the collection container 7.

When the circulation path is formed along the main path as described above and the adsorption vessel 5 is provided, the fluid is prevented from being saturated by the dissolution of the extracted component, and the extraction efficiency is always high (a large extracted component). Volume and short extraction time). In addition, since a predetermined amount of fluid can be repeatedly supplied to the extraction step through the circulation system for extraction, the amount of fluid used can be reduced, and the process environment is improved.

At this time, the completion of the extraction operation can be clearly recognized by monitoring the extraction status by the detector 4 (for example, monitoring the detection data of a detector composed of a spectrophotometer). Therefore, unnecessary working time is eliminated.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing a configuration of a supercritical fluid extraction device according to an embodiment of the present invention.

FIG. 2 is a schematic diagram showing a configuration of a supercritical fluid extraction device according to a conventional example.

[Explanation of symbols]

1 is a fluid cylinder, 2 is a pressure pump, 3 is an extraction vessel, 4 is a detector, 5 is an adsorption vessel, 6 is a pressure control device, 7 is a recovery vessel, 8 is a first switching valve, and 9 is a second switching valve. Switching valve, 1
0 is a circulation pump and 11 is a temperature control device.

 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Tadahiro Takahachi 2217-2 Hayashi-cho, Takamatsu-shi, Kagawa Prefecture Ryusho Sangyo Co., Ltd. Research Information Center F term (reference) 4D056 AC24 BA16 CA33 CA34 CA36 CA40 DA01 DA02

Claims (1)

[Claims] 1. A supercritical fluid extraction device for extracting a desired component from a predetermined sample substance in a supercritical state of a predetermined fluid, comprising: a pressure pump, an extraction container, a detector, an adsorption container, and a pressure control device. And a switching valve is provided at each of the inlet pipe of the extraction vessel and the outlet pipe of the adsorption vessel, and the switching valves are connected to each other by a pipe and circulated in the middle of the pipe. A supercritical fluid extraction device, wherein a pump is provided, and the switching valve is switched to form a circulation path from the adsorption container to the extraction container.