JPH0321302A - Extraction and separation device - Google Patents

Abstract

PURPOSE:To enable recovery of a specified component in high concentration by providing two separation sections or more for fractionating extracted components and also providing a concentration section for concentrating specified components fractionated by the separation sections further to higher degree. CONSTITUTION:An extraction section A for extracting components to from a raw material by introducing supercritical fluid and separation sections B1 and B2 for fractionating the supercritical fluid and the components are provided. Two separation sections B1, B2 or more for fractionating the components to be extracted are juxtaposed, and a concentration section C for the purpose concentrating specified components and fractionated by the separation sections further to higher degree is provided. The concentrations section C consists of re-extraction tank 31 and two-re-separation tanks 32 and 33, and the re- extraction tank 31 is connected respectively with the re-separation tanks 32 and 33 through pressure control valves 36c and 36d. As a result, only the aimed specified components can be recovered in high concentration.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a separation device that recovers extracted components using a solvent. This invention relates to an extraction separation device that can be recovered.

[Prior Art] Extraction and separation devices are used to extract specific components, such as fragrance components and oil and fat components, from natural animals and plants, or to purify pharmaceutical products. The supercritical extraction method used is attracting attention, ′! Figure J3 is a schematic explanatory diagram showing an example of a supercritical extraction separation device.

The extraction separation device 1 includes an extraction section A. The main parts are the separation part B and the CO2 supply part D, and the CO2 of the CO2 supply part D is
The C02 gas supplied from the tank 10 is liquefied in the liquefier 11, then pressurized in the pump 14, further heated and pressurized in the heat exchanger 15, and introduced into the extraction tank 22 constituting the extraction section A as a supercritical fluid. Ru. On the other hand, raw materials are supplied to the extraction tank 22 from a raw material supply device 21,
The supercritical fluid that has come into contact with the raw material extracts dissolved components from the raw material, and the liquid CO containing the dissolved components is sent to the separation tank 23 constituting the separation section B. In the separation tank 23, a specific component is separated from the dissolved components by adjusting the pressure and temperature, and the specific component is stored in the extraction tank 24.

Then, unnecessary dissolved components and liquid CO2 are introduced into the vaporization tank 25? The temperature is increased to gasify the liquid CO2, which is sent to the liquefier 11 through the cooler 26, where the CO2 is circulated and reused, and unnecessary components are stored in the lower part of the vaporization tank 25 and discharged as appropriate.

[Problems to be Solved by the Invention] By the way, the dissolved components extracted from the raw materials in the extraction process 22 are rarely composed of only a single pure component, and are usually a mixture of multiple types of components. many. That is, when natural animals and plants are used as raw materials, many components with similar chemical structures are included, so these similar components are dissolved in parallel in the supercritical fluid (liquid CO2). Moreover, it is very difficult to separate only a specific component from these mixed components in the separation section B, and a plurality of components having similar chemical structures are collected in the extraction tank 24 in a mixed state, and the concentration of the target component is You can't expect much to get it in a high state.

Although it is theoretically possible to control pressure and temperature conditions in the separation tank 23 to separate specific components to be recovered, it would increase costs in terms of equipment and management, making it impractical for actual operation. Not suitable. Therefore, the present inventors conducted extensive research and completed the present invention with the aim of providing an extraction and separation device that can recover only a specific target component at a high concentration even in such a case C.

[A Thousand Steps to Solve the Problems] The present invention, which has achieved the above object, has two or more separation sections for fractionating the extracted components, and a specific recovery purpose separated by the separation section. The gist of this is that it is equipped with a concentrating section to further increase the concentration of the components.

[Operations and Examples] FIG. 1 is a schematic explanatory diagram showing a typical example of the present invention. The extraction separation device includes an extraction section A, two separation sections Bl. B
The extraction tank 22, which has the main parts of the extraction tank 2 and the concentrating part C, and which is connected to the extraction part A, is connected to the separation tanks 23a and 23b, which constitute the two separation parts Bl and B2, through pressure control valves 36a and 36b, respectively. The pressure in the extraction tank 22 is adjusted by one of the pressure control valves 36a, 36b, and the pressure in the separation tanks 23a, 23b is adjusted by the pressure adjustment valves 37a, 37b. ．． Further, the temperature of the extraction tank 22, separation tanks 23a, 23b, etc. can be adjusted to a predetermined temperature using a heat medium.

On the other hand, the CO2 gas supplied from the CO2 supply section D is cooled and liquefied in the condenser 38, pressurized by the pressurizing pump 35a, and then heated and heated by the heat exchanger 34 so that it can be supplied to the extraction tank 22 as a supercritical fluid. configured.

In addition, the concentration section C is connected to the separation tank 23a via an intermediate tank 30.
is connected. The concentration section C consists of a re-extraction tank 31 and two re-separation tanks 32, 33, and the re-extraction tank 31 has a pressure control valve 36c. It is connected to reseparation tanks 32 and 33 via 36d, respectively.

An example of separating and recovering yellow pigments from crushed chili peppers using the extraction separation device with the above configuration will be explained below. Extraction 4! Raw materials are supplied into 22, and supercritical liquid C is added to this.
When O2 is introduced, the precepts are extracted from the raw material with a concentration distribution as shown in Figure 2. Ta. That is, at the initial stage of extraction (to onet +
In the latter half of the extraction period (1+
-t2) shows an extraction distribution centered on the red pigment group (peak G in the figure). Therefore time t
The liquid CO2 at the early stage of extraction is introduced into the separation section Bl, while the liquid CO2 at the latter stage of the extraction is introduced into the separation section B2. In this embodiment, the initial stage of extraction at high pressure and the latter stage of extraction at low pressure are controlled by the pressure control valve 36a. 36b, as selectively switched by
The set pressures of the valves 36a and 36b are changed. In addition, a configuration in which the flow path of liquid CO2 is changed by a timer may also be used. In other words, liquid CO2 containing yellow pigments at the initial stage of extraction.
is introduced into the separation column 23a, and the liquid CO2 containing the red pigment group in the latter stage of extraction is introduced into the separation column 23b. i
The dye group and liquid CO2 are separated by adjusting the pressure and temperature in the ll tanks 23a and 23b. Although the above example shows an example of separation based on a pressure difference and a time difference, it goes without saying that a separation technique using other factors can be adopted.

The yellow pigment group separated in the above separation 4g 2 3 B has a high β-carotene concentration, and is further subjected to the following treatment in the concentration section C.

That is, the extracted ingredients in the intermediate tank 30 are introduced into the re-extraction tank 31 by the transfer bomb 35b, and the pressurized bomb 35
The liquid CO2 pressurized by a is heated in the heat exchanger 34 and introduced into the re-extraction tank 31 as supercritical liquid CO2, and in the same manner as the above-mentioned separation section "l + 82", the re-separation S tank is used at the initial stage of extraction. 32 to separate and collect the oily components,
In the latter stage of the extraction, it is fed to the re-separation tank 33 and the yellow pigment group with low β-carotene concentration is recovered in re-separation@4!33. Note that the branching to the re-separation tanks 32 and 33 in this re-extraction step may be performed by using the pressure control valves 36c and 36d as in the previous example, or by using a branch valve equipped with a timer. good.

In the example shown in FIG. 1, the re-extraction tank 31 and the re-separation tank 32 are connected via a transfer pump 35c, and are configured to increase the concentration of the yellow pigment group in the oily component without wasting it. .

The operating temperature in the extraction separation device is 40 to 100°C, and the operating pressure in the extraction section is 200 to 800 kg/c.
m2, the operating pressure of separation section B,, B, is normal pressure to 100
kg/cm', the operating pressure of concentration section C is 150-50
0 kg/cm", but these are only examples and do not limit the present invention. The above subdivision l!!4!33
The group of yellow pigments that are separated can be recovered in high concentrations with less contamination by similar components. Note that the concentration section C may use a chromatography device instead of the re-extraction structure.

The CO2 discharged from the separation tanks 23a, 23b and the separation tanks 32, 33 is collected in the gas purification device 26, and after separating and purifying the mixed unpleasant odor components, it is circulated to the condenser 38 and recycled. used.

The apparatus of the present invention is not limited to the above-mentioned embodiment, and the number of separation sections can be arbitrarily set as long as there are two or more, and a plurality of concentration sections C can also be provided.

[Effects of the Invention] Since the present invention is configured as described above, it has become possible to purify and recover a specific target component to be recovered at a high concentration.

[Brief explanation of the drawing]

Fig. 1 is a schematic explanatory diagram showing a typical embodiment of the present invention, Fig. 2 is a graph showing the distribution of extracted components in the separation section, and Fig. 3 is a schematic explanatory diagram showing an example of a conventional extraction and separation device. be. 1... Extraction separation device 2... C O 2 tank 2
...tlW converter 13...filter 14
... Pressure pump 15 ... Heat exchanger 21 ... Raw material supply device 22 ... Extraction tank 23, 23a, 23b.
-Separation tank 24...Extraction tank 25...Vaporization tank 26-
・・Reliever 30 ・Intermediate tank 31 ・Re-extraction tank 32.33 ・Re-separation m tank 34 ・Heat exchangers 36a to 36d ・Pressure control valves 37a, 37b... Pressure regulating valve 38... capacitor

Claims (1)

[Claims] An extraction and separation device comprising an extraction section for introducing a supercritical fluid to extract extracted components from a raw material, and a separation section for separating the supercritical fluid and the extracted components, the separation device for fractionating the extracted components. An extraction and separation apparatus characterized by having two or more parts in parallel and a concentrating part for further increasing the concentration of a specific target component to be recovered that has been separated by the separating part.