CN220656479U - Separation rectifying device for supercritical extraction process - Google Patents

Separation rectifying device for supercritical extraction process Download PDF

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Publication number
CN220656479U
CN220656479U CN202320769968.5U CN202320769968U CN220656479U CN 220656479 U CN220656479 U CN 220656479U CN 202320769968 U CN202320769968 U CN 202320769968U CN 220656479 U CN220656479 U CN 220656479U
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rectifier
separation
gas
kettle
liquid separator
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吕金杰
于群
吕磊
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Harbin Essence Biotechnology Co ltd
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Harbin Essence Biotechnology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The utility model provides a separation rectifying device for a supercritical extraction process, and belongs to the field of supercritical extraction processes. Solves the problem that the conventional supercritical extraction equipment can not effectively separate the components. The device comprises a separation kettle, a gas-liquid separator and a rectifier, wherein the rectifier is arranged inside the separation kettle, a rectifier top plate and a rectifier bottom plate are respectively arranged at the top and the bottom of the rectifier, the rectifier top plate and the rectifier bottom plate are respectively arranged at intervals with the top and the bottom of the separation kettle, the gas-liquid separator is arranged at the top of the inside of the rectifier, the top of the gas-liquid separator is connected with the rectifier top plate, a pressurizing bottom plate is arranged at the bottom of the gas-liquid separator, a gas-liquid separation pipe is arranged in the gas-liquid separator, one end of the gas-liquid separation pipe penetrates through the side walls of the top of the rectifier top plate and the top of the separation kettle, and the other end of the gas-liquid separation pipe extends to the bottom of an inner cavity of the gas-liquid separator. It is mainly used for separation and rectification in supercritical extraction process.

Description

Separation rectifying device for supercritical extraction process
Technical Field
The utility model belongs to the field of supercritical extraction technology, and particularly relates to a separation rectifying device of the supercritical extraction technology.
Background
Supercritical fluid (SCF) refers to a fluid in a particular state in which a substance is at or above its critical temperature and critical pressure. Supercritical fluid extraction is the extraction of specific components from liquids or solids using a fluid under supercritical conditions as an extractant.
Supercritical extraction is divided into two main process sections of extraction and separation. In the extraction process section, a fluid medium in a supercritical state at a set pressure and temperature is used for dissolving out substance components in the materials; in the separation process section, the supercritical fluid is separated by changing the pressure and temperature so that the solubility of the extract substance in the supercritical medium is reduced.
Supercritical extraction is theoretically effective in separating substances with large molecules, small molecules, different polarities and different solubilities through changes in pressure and temperature. However, in practice, the solubility is reduced and the components are rapidly separated, so that the components cannot be well separated, and the effect of separating the components cannot be achieved.
The conventional supercritical extraction equipment separation process section is generally provided with two to three separation kettles, the separation kettles are in a serial structure, the pressure is reduced, and different temperature controls are combined, so that the dissolution capacity of supercritical fluid media is changed, gradient separation of the extract and the supercritical media in each separation kettle is realized, the separation kettles are in a serial structure, the dissolution capacity of the supercritical media is reduced due to the change of the temperature and the pressure, solutes of different components in the extract are separated out and separated together due to the reduction of the solubility, and the extract is not separated out and enters the next separation kettle for separation. The various components of the precipitated extract were mixed together and not effectively separated.
The other type of separation device is a rectification column, which is generally divided into 3-5 sections of separation columns, the separation columns are connected in series from bottom to top, the pressure is the same, the dissolution capacity is changed by changing the temperature, so that the separation of components is realized, the structure of the rectification column is small in the solubility change range of a supercritical medium due to the volume of the column and the adjustment of a single temperature parameter, the separation capacity and the treatment capacity are limited, and the application is not more in practical production.
Disclosure of Invention
In view of the above, the present utility model aims to provide a separation rectifying device for supercritical extraction process, so as to solve the problem that conventional supercritical extraction equipment cannot effectively separate components.
In order to achieve the above purpose, the present utility model adopts the following technical scheme: the utility model provides a separation distillation plant of supercritical extraction technology, it includes separation cauldron, vapour and liquid separator and rectifier, the rectifier sets up inside the separation cauldron, the top and the bottom of rectifier are equipped with rectifier roof and rectifier bottom plate respectively, rectifier roof and rectifier bottom plate set up with the top and the bottom interval of separation cauldron respectively, vapour and liquid separator sets up at the inside top of rectifier, vapour and liquid separator's top is connected with the rectifier roof, vapour and liquid separator's bottom is equipped with the pressure boost bottom plate, be equipped with the gas-liquid separation pipe in the vapour and liquid separator, the lateral wall setting at rectifier roof and separation cauldron top is passed to the one end of gas-liquid separation pipe, the other end extends to the bottom of vapour and liquid separator inner chamber, the separation cauldron outside is through vapour and liquid separation pipe and vapour and liquid separator inner chamber intercommunication, be provided with the air duct in the rectifier, the air inlet end of air duct extends to the upper half of vapour and liquid separator inner chamber, and the air outlet end of air duct passes the pressure boost bottom plate and rectifier bottom plate setting, be provided with the gas outlet on the rectifier roof, the gas outlet passes through the rectifier inner chamber of rectifier and rectifier inner chamber and the top intercommunication.
Further, a separation kettle pressure cap plug is arranged at the top end of the separation kettle.
Still further, the bottom of separation cauldron is provided with the material valve that connects, the inner chamber of separation cauldron bottom is through material valve and separation cauldron outside intercommunication.
Furthermore, the inner cavities of the gas-liquid separator and the rectifier are provided with filling materials.
Furthermore, a plurality of small holes are formed in the bottom plate of the rectifier and the pressurizing bottom plate.
Furthermore, a plurality of rectifier support legs are arranged in the inner cavity at the bottom of the separation kettle, and the rectifier bottom plate is connected with the separation kettle through the rectifier support legs.
Furthermore, a supercritical medium outlet is arranged on the side wall of the top of the separation kettle, and an inner cavity of the top of the separation kettle is communicated with the outside of the separation kettle through the supercritical medium outlet.
Furthermore, a supercritical gas-liquid mixing inlet is further formed in the side wall of the top of the separation kettle, and one end of the gas-liquid separation pipe is connected with the supercritical gas-liquid mixing inlet.
Further, a filter screen is arranged at the air inlet of the air duct.
Further, a sealing ring is arranged between the top of the gas-liquid separator and the top plate of the rectifier.
Compared with the prior art, the utility model has the beneficial effects that:
1. the utility model realizes the integration of separation and rectification by designing the structures of the gas-liquid separator and the rectifier in the original separation kettle;
2. the utility model combines separation and rectification together, so that the separated supercritical fluid medium is extracted with the extract liquid again, and the substance components in the extract can be effectively separated, thereby realizing the rectification purpose;
3. the utility model combines separation and rectification in the same working section, utilizes pressure and temperature change to realize the rapid separation of supercritical fluid medium and extract, and the extract liquid flows through a rectifier from top to bottom, and the separated supercritical fluid medium passes through the rectifier from bottom to top, and light components (small molecules and low polarity) in the separated extract are redissolved in the rectifier, and heavy components (macromolecules and high polarity) in the supercritical fluid medium are separated, thereby realizing the purpose of separating substance components;
4. according to the utility model, the gas-liquid separator enables the internal pressure to be slightly higher than that of the rectifier through the pressurizing bottom plate, so that the extract liquid can be uniformly sprayed on the packing of the rectifier during one-time separation.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model. In the drawings:
fig. 1 is a schematic diagram of the whole structure of a separation rectifying device of a supercritical extraction process according to the present utility model.
The device comprises a 1-separation kettle, a 2-rectifier, a 3-gas-liquid separator, a 4-gas-liquid separation pipe, a 5-gas guide pipe, a 6-rectifier top plate, a 7-rectifier bottom plate, an 8-pressurizing bottom plate, a 9-sealing ring, a 10-filter screen, a 11-supercritical gas-liquid mixing inlet, a 12-supercritical medium outlet, a 13-separation kettle pressure cap plug, a 14-rectifier gas outlet, a 15-filler, 16-rectifier supporting legs and a 17-receiving valve.
Detailed Description
The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. It should be noted that, in the case of no conflict, embodiments of the present utility model and features of the embodiments may be combined with each other, and the described embodiments are only some embodiments of the present utility model, not all embodiments.
Referring to fig. 1 for illustrating the present embodiment, a separation and rectification device for supercritical extraction process includes a separation tank 1, a gas-liquid separator 3 and a rectifier 2, the rectifier 2 is disposed inside the separation tank 1, a top and a bottom of the rectifier 2 are respectively provided with a rectifier top plate 6 and a rectifier bottom plate 7, the rectifier top plate 6 and the rectifier bottom plate 7 are respectively disposed at intervals between the top and the bottom of the separation tank 1, the gas-liquid separator 3 is disposed at the top of the inside of the rectifier 2, the top of the gas-liquid separator 3 is connected with the rectifier top plate 6, a pressurizing bottom plate 8 is disposed at the bottom of the gas-liquid separator 3, a gas-liquid separation tube 4 is disposed in the gas-liquid separator 3, one end of the gas-liquid separation tube 4 passes through the side walls of the top plate 6 and the top of the separation tank 1, the other end extends to the bottom of an inner cavity of the gas-liquid separator 3, an air duct 5 is disposed in the separator 2, the air duct 5 extends to the top of the inner cavity of the gas-liquid separator 3, and the gas outlet 14 is disposed at the top of the rectifying tank 1, and the top of the gas duct 5 passes through the top plate 6, and the pressurizing bottom plate 14 is disposed at the top of the rectifying bottom plate 1.
In the embodiment, a rectifier top plate 6 and a rectifier bottom plate 7 are connected with the rectifier 2 through screws, an air duct 5 is welded and sealed with a pressurizing bottom plate 8, and a gas-liquid separator 3 is welded and sealed with the rectifier top plate 6.
In the embodiment, the structure of the gas-liquid separator 3 and the rectifier 2 in the original separation kettle 1 is designed, so that the separation and rectification integration is realized.
The embodiment combines separation and rectification together, so that the separated supercritical fluid medium is subjected to secondary extraction with the extract liquid again, and substance components in the extract can be effectively separated, thereby achieving the purpose of rectification.
In the embodiment, separation and rectification are combined in the same working section, the rapid separation of the supercritical fluid medium and the extract is realized by utilizing the pressure and temperature change, the extract liquid flows through the rectifier 2 from top to bottom, the separated supercritical fluid medium passes through the rectifier 2 from bottom to top, the light components (small molecules and low polarity) in the separated extract are redissolved in the rectifier 2 into the supercritical fluid medium, and the heavy components (macromolecules and high polarity) in the supercritical fluid medium are separated, so that the purpose of separating the substance components is realized.
In this embodiment, a separation kettle pressure cap plug 13 is disposed at the top end of the separation kettle 1, and the separation kettle pressure cap plug 13 is used for sealing the separation kettle 1.
In this embodiment, the bottom end of the separation kettle 1 is provided with a receiving valve 17, and the inner cavity at the bottom of the separation kettle 1 is communicated with the outside of the separation kettle 1 through the receiving valve 17, and the receiving valve 17 can periodically discharge the temporarily stored extract at the bottom of the separation kettle 1.
In this embodiment, the inner cavities of the gas-liquid separator 3 and the rectifier 2 are both provided with a filler 15, in this embodiment, the surface of the filler 15 is net-shaped, and the separated supercritical fluid medium has a plurality of separated extract tiny droplets suspended therein, and larger droplets are gradually formed by contacting with the filler 15 and collected in the extract liquid.
In this embodiment, the rectifier bottom plate 7 and the pressurizing bottom plate 8 are provided with a plurality of small holes, and the rectifier bottom plate 7 and the pressurizing bottom plate 8 are provided with small holes for the circulation of the extract liquid.
In this embodiment, a plurality of rectifier legs 16 are disposed in the inner cavity at the bottom of the separation kettle 1, the rectifier bottom plate 7 is connected with the separation kettle 1 through the plurality of rectifier legs 16, and the rectifier legs 16 are used for supporting the rectifier 2 in the separation kettle 1, and make the bottom of the separation kettle 1 have enough space to temporarily store the extract liquid.
In this embodiment, a supercritical medium outlet 12 is disposed on a side wall of the top of the separation kettle 1, an inner cavity of the top of the separation kettle 1 is communicated with the outside of the separation kettle 1 through the supercritical medium outlet 12, and a supercritical fluid medium subjected to secondary rectification enters the inner cavity of the top of the separation kettle 1 through a rectifier air outlet 14 and flows out of the separation kettle 1 through the supercritical medium outlet 12 of the separation kettle 1.
In this embodiment, a supercritical gas-liquid mixing inlet 11 is further provided on a side wall of the top of the separation kettle 1, one end of the gas-liquid separation tube 4 is connected with the supercritical gas-liquid mixing inlet 11, and the mixed solution of the supercritical fluid medium and the extract enters the gas-liquid separator 3 through the gas-liquid separation tube 4 from the supercritical gas-liquid mixing inlet 11.
In this embodiment, the air inlet of the air duct 5 is provided with a filter screen 10, and in this embodiment, the filter screen 10 is made of stainless steel.
In this embodiment, a sealing ring 9 is disposed between the top of the gas-liquid separator 3 and the top plate 6 of the rectifier, and the sealing ring 9 is used to ensure tightness between the gas-liquid separator 3 and the top plate 6 of the rectifier.
The working principle of this embodiment is as follows:
the mixed solution of the supercritical fluid medium and the extract enters the gas-liquid separator 3 through the gas-liquid separation pipe 4 from the supercritical gas-liquid mixing inlet 11, the supercritical fluid and the extract liquid are rapidly separated in the gas-liquid separator 3, a plurality of separated fine droplets of the extract are suspended in the supercritical fluid medium after separation, larger droplets are gradually formed by contacting with the packing 15 in the gas-liquid separator 3, the large droplets are collected in the extract liquid, the separated supercritical fluid medium enters the gas-liquid through the gas inlet of the gas-guide pipe 5 positioned at the upper half of the gas-liquid separator 3 and is led out from the gas outlet of the gas-guide pipe 5 positioned at the lower half of the rectifier 2, the extract liquid is uniformly sprayed onto the packing 15 in the rectifier 2 through small holes formed in the pressurizing bottom plate 8 of the gas-liquid separator 3, the supercritical fluid medium gradually gathers along the net surface of the packing 15 from top to the inner cavity below the rectifier bottom plate 7, the supercritical fluid medium discharged from the gas outlet of the gas-guide pipe 5 flows through the rectifier 2 from top to the inner cavity of the rectifier 1, the extract liquid distributed on the surface of the top of the rectifier 15 and the extract liquid is discharged from the supercritical fluid medium 1 through the top of the separator 1 through the buffer valve 1 at the top of the rectifier 1 at the time of the buffer 1 is separated from the buffer 1.
The embodiments of the utility model disclosed above are intended only to help illustrate the utility model. The examples are not intended to be exhaustive or to limit the utility model to the precise forms disclosed. Many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the utility model and the practical application, to thereby enable others skilled in the art to best understand and utilize the utility model.

Claims (10)

1. A separation rectifying device of a supercritical extraction process is characterized in that: the utility model comprises a separating kettle (1), a gas-liquid separator (3) and a rectifier (2), wherein the rectifier (2) is arranged inside the separating kettle (1), a top and a bottom of the rectifier (2) are respectively provided with a rectifier top plate (6) and a rectifier bottom plate (7), the top and the bottom of the rectifier top plate (6) and the rectifier bottom plate (7) are respectively arranged at intervals with the top and the bottom of the separating kettle (1), the gas-liquid separator (3) is arranged at the top inside the rectifier (2), the top of the gas-liquid separator (3) is connected with the rectifier top plate (6), the bottom of the gas-liquid separator (3) is provided with a pressurizing bottom plate (8), one end of the gas-liquid separator (4) passes through the side wall of the top of the rectifier top plate (6) and the separating kettle (1), the other end of the gas-liquid separator extends to the bottom of an inner cavity of the gas-liquid separator (3), the outer part of the separating kettle (1) passes through the gas-liquid separator (4) and the gas guide tube (3) to the inner cavity (5), the gas-liquid separator (3) is provided with a gas guide tube (5) and the gas-guide tube (5) is arranged at the bottom of the gas-guide tube (5), the top plate (6) of the rectifier is provided with a rectifier air outlet (14), and the inner cavity of the rectifier (2) is communicated with the inner cavity at the top of the separation kettle (1) through the rectifier air outlet (14).
2. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: the top end of the separation kettle (1) is provided with a separation kettle pressure cap plug (13).
3. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: the bottom of the separation kettle (1) is provided with a material receiving valve (17), and an inner cavity at the bottom of the separation kettle (1) is communicated with the outside of the separation kettle (1) through the material receiving valve (17).
4. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: and the inner cavities of the gas-liquid separator (3) and the rectifier (2) are provided with filling materials (15).
5. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: a plurality of small holes are formed in the rectifier bottom plate (7) and the pressurizing bottom plate (8).
6. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: a plurality of rectifier support legs (16) are arranged in an inner cavity at the bottom of the separation kettle (1), and the rectifier bottom plate (7) is connected with the separation kettle (1) through the rectifier support legs (16).
7. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: the supercritical medium separation device is characterized in that a supercritical medium outlet (12) is formed in the side wall of the top of the separation kettle (1), and an inner cavity of the top of the separation kettle (1) is communicated with the outside of the separation kettle (1) through the supercritical medium outlet (12).
8. The separation and rectification apparatus of a supercritical extraction process of claim 7, wherein: the side wall of the top of the separation kettle (1) is also provided with a supercritical gas-liquid mixing inlet (11), and one end of the gas-liquid separation pipe (4) is connected with the supercritical gas-liquid mixing inlet (11).
9. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: a filter screen (10) is arranged at the air inlet of the air duct (5).
10. The separation and rectification apparatus of a supercritical extraction process of claim 1, wherein: a sealing ring (9) is arranged between the top of the gas-liquid separator (3) and the top plate (6) of the rectifier.
CN202320769968.5U 2023-04-10 2023-04-10 Separation rectifying device for supercritical extraction process Active CN220656479U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202320769968.5U CN220656479U (en) 2023-04-10 2023-04-10 Separation rectifying device for supercritical extraction process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202320769968.5U CN220656479U (en) 2023-04-10 2023-04-10 Separation rectifying device for supercritical extraction process

Publications (1)

Publication Number Publication Date
CN220656479U true CN220656479U (en) 2024-03-26

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CN202320769968.5U Active CN220656479U (en) 2023-04-10 2023-04-10 Separation rectifying device for supercritical extraction process

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