CN116371000A - Processing system for extracting plant active ingredient by supercritical fluid and control method - Google Patents
Processing system for extracting plant active ingredient by supercritical fluid and control method Download PDFInfo
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- CN116371000A CN116371000A CN202310315471.0A CN202310315471A CN116371000A CN 116371000 A CN116371000 A CN 116371000A CN 202310315471 A CN202310315471 A CN 202310315471A CN 116371000 A CN116371000 A CN 116371000A
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- 239000012530 fluid Substances 0.000 title claims abstract description 278
- 239000004480 active ingredient Substances 0.000 title claims abstract description 68
- 238000012545 processing Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 34
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 540
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 270
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 270
- 238000000605 extraction Methods 0.000 claims abstract description 195
- 238000001816 cooling Methods 0.000 claims abstract description 76
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 55
- 238000000746 purification Methods 0.000 claims abstract description 48
- 238000009833 condensation Methods 0.000 claims abstract description 42
- 230000005494 condensation Effects 0.000 claims abstract description 42
- 238000005194 fractionation Methods 0.000 claims abstract description 42
- 230000008016 vaporization Effects 0.000 claims abstract description 31
- 238000007906 compression Methods 0.000 claims abstract description 22
- 230000006835 compression Effects 0.000 claims abstract description 22
- 238000009834 vaporization Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims description 226
- 239000000463 material Substances 0.000 claims description 212
- 239000007788 liquid Substances 0.000 claims description 69
- 239000000284 extract Substances 0.000 claims description 42
- 238000004821 distillation Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000004891 communication Methods 0.000 claims description 7
- 238000004508 fractional distillation Methods 0.000 claims description 4
- 238000005265 energy consumption Methods 0.000 abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 70
- 230000001276 controlling effect Effects 0.000 description 49
- 238000012546 transfer Methods 0.000 description 31
- 241000196324 Embryophyta Species 0.000 description 23
- 238000010586 diagram Methods 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000005057 refrigeration Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000012071 phase Substances 0.000 description 2
- 230000005514 two-phase flow Effects 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 240000001140 Mimosa pudica Species 0.000 description 1
- 235000016462 Mimosa pudica Nutrition 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
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- 239000001294 propane Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
- B01D11/0296—Condensation of solvent vapours
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a processing system for extracting plant active ingredients by supercritical fluid and a control method, wherein the processing system comprises a supercritical fluid extraction subsystem, a fractionation purification subsystem and a carbon dioxide cold and heat combined supply subsystem; the supercritical fluid extraction subsystem is connected in series with the fractionation purification subsystem. The supercritical fluid extraction subsystem comprises a first fluid branch and a second fluid branch connected in series; the fractionation purification subsystem comprises a vaporization part and a condensation part; the carbon dioxide cold and hot combined supply subsystem comprises a compression unit, a first heat supply unit, a second heat supply unit, a first cooling unit and a second cooling unit; the first cooling unit exchanges heat with the first fluid branch; the second heat supply unit exchanges heat with the second fluid branch; the first heat supply unit exchanges heat with the vaporization part, and the second cooling unit exchanges heat with the condensation part. The processing system and the control method realize high-efficiency and high-purity extraction of effective substances and low-energy-consumption operation.
Description
Technical Field
The invention relates to the technical field of extraction of plant active ingredients, in particular to a processing system for extracting plant active ingredients by supercritical fluid and a control method.
Background
The active ingredients in plants, such as essential oils, have very wide application in the pharmaceutical, food, cosmetic and perfume industries. The extraction method of the plant active ingredients comprises distillation, solvent extraction, soxhlet extraction, compression, water distillation and the like, but the methods have the defects of long extraction time, large consumption of organic solvents, large loss of volatile substances, poor thermal stability, possible residual toxic solvents in the extract, low yield, low extraction efficiency and the like.
In the related art, with the development of the deep-processing technology, the supercritical fluid extraction technology is gradually becoming the most preferred method for extracting and separating the effective components from plants. The principle is that the active ingredients are separated and purified by utilizing the characteristic that the fluid has selective dissolving capability on substances in a supercritical state, and the method has the advantages of good separation effect, high quality, high yield, environmental protection and the like, and is suitable for extracting the active ingredients in heat-sensitive plants such as flowers and the like. However, because of the extremely strong dissolving capacity of the supercritical fluid and the particularity of the plant itself, some other natural compounds, such as some waxes, are extracted at the same time when the supercritical fluid is used for extracting the plant active ingredients, so that the purity of the plant active ingredients extracted by the traditional supercritical fluid extraction process is low, and meanwhile, the supercritical fluid extraction process has the requirements of heating and cooling at the same time, and the energy consumption for independently heating and cooling the supercritical fluid is high.
Disclosure of Invention
The invention aims to at least solve the problems of low purity and high energy consumption of the supercritical fluid extraction of plant active ingredients. The aim is achieved by the following technical scheme:
the first aspect of the invention provides a processing system for extracting plant active ingredients by supercritical fluid, which comprises a supercritical fluid extraction subsystem, a fractionation purification subsystem and a carbon dioxide cold and hot combined supply subsystem; wherein,,
the supercritical fluid extraction subsystem is used for separating a first material containing active ingredients from a material to be extracted by utilizing supercritical carbon dioxide; the supercritical fluid extraction subsystem comprises a first fluid branch and a second fluid branch which are connected in series along the flow direction of the carbon dioxide;
the fractionation purification subsystem is connected in series with the second fluid branch and is used for purifying the effective components in the first material; the fractionation purification subsystem comprises a vaporization part and a condensation part;
the carbon dioxide cold and hot combined supply subsystem comprises a compression unit, a first heat supply unit, a second heat supply unit, a first cooling unit and a second cooling unit; the compression unit, the first heat supply unit and the second heat supply unit are sequentially connected in series along the flowing direction of carbon dioxide; the first cooling unit and the second cooling unit are connected in parallel, an inlet of a parallel passage of the first cooling unit and the second cooling unit is communicated with the second heat supply unit, and an outlet of a parallel passage of the first cooling unit and the second cooling unit is communicated with the compression unit;
The first cooling unit exchanges heat with the first fluid branch so as to condense gaseous carbon dioxide in the first fluid branch into liquid carbon dioxide; the second heat supply unit exchanges heat with the second fluid branch so as to heat supercritical carbon dioxide in the second fluid branch to reach a preset extraction temperature or separation temperature; the first heat supply unit is in heat exchange with the vaporizing part so as to vaporize the effective components in the first material entering the vaporizing part; and the second cooling unit is in heat exchange with the condensing part so as to condense the vaporized active ingredients.
According to the processing system, the supercritical fluid extraction subsystem and the fractional distillation purification subsystem are operated at proper temperatures by arranging the carbon dioxide cold and hot combined supply subsystem, so that other unwanted compounds in plants are prevented from being extracted, and the purity of active ingredients is improved. Meanwhile, heat supply and refrigeration respectively generate energy consumption in the traditional supercritical fluid extraction process, and the carbon dioxide cold and hot combined supply subsystem can realize heat supply and refrigeration simultaneously under the same energy consumption, so that the energy consumption of a processing system is reduced.
In addition, the processing system according to the invention may have the following additional technical features:
in some embodiments of the invention, the supercritical fluid extraction subsystem comprises a to-be-extracted storage tank, a gaseous fluid storage tank, a first heat exchange device, a gas-liquid separation tank, a liquid fluid storage tank, an extraction separation unit, a gaseous fluid separation tank, and a first material storage tank; the gaseous fluid storage tank, the first heat exchange device, the gas-liquid separation tank and the liquid fluid storage tank are sequentially connected in series on the first fluid branch along the flowing direction of carbon dioxide; the gaseous fluid outlet of the gas-liquid separation tank is communicated with the fluid inlet of the first heat exchange device; the extraction separation unit is arranged on the second fluid branch, and the storage tank for the to-be-extracted matters is communicated with the material inlet of the extraction separation unit; the material outlet of the extraction separation unit is communicated with the gaseous fluid separation tank, and the material outlet of the gaseous fluid separation tank is communicated with the first material storage tank; the fluid outlet of the extraction separation unit and the fluid outlet of the gaseous fluid separation tank are communicated with the outlet of the gaseous fluid storage tank;
The first cooling unit comprises a first throttling expansion device and a first carbon dioxide storage tank which are connected in series, a fluid inlet of the first throttling expansion device is communicated with the second heating unit, and a fluid outlet of the first carbon dioxide storage tank is communicated with the compression unit; and a first carbon dioxide circulation loop is formed between the first carbon dioxide storage tank and the first heat exchange device.
In some embodiments of the invention, the extraction separation unit comprises an extraction kettle, at least one separation kettle and a plurality of second heat exchange devices, wherein the extraction kettle is connected with the at least one separation kettle in series along the flow direction of carbon dioxide, and the plurality of second heat exchange devices are respectively arranged at fluid inlets of the extraction kettle and the at least one separation kettle; the material outlet of the storage tank for the to-be-extracted substances is communicated with the material inlet of the extraction kettle; the material outlet of the separation kettle is communicated with the gaseous fluid separation tank, and the fluid outlet of the separation kettle is communicated with the outlet of the gaseous fluid storage tank; an evacuation pipeline is arranged at the bottom of the extraction kettle;
the second heat supply unit comprises a plurality of third heat exchange devices and a plurality of first heat exchange medium storage devices, and the third heat exchange devices are connected in series; the third heat exchange device is arranged corresponding to the first heat exchange medium storage device, and the first heat exchange medium storage device is arranged corresponding to the second heat exchange device; a first heat exchange medium circulation loop is formed between the third heat exchange device and the corresponding first heat exchange medium storage device, and a second heat exchange medium circulation loop is formed between the first heat exchange medium storage device and the corresponding second heat exchange device.
In some embodiments of the present invention, the processing system includes a plurality of the extraction separation units, the plurality of extraction separation units are connected in parallel, the material outlet of the storage tank for the material to be extracted is respectively communicated with the material inlets of the plurality of extraction separation units, the material outlets of the plurality of extraction separation units are respectively communicated with the gaseous fluid separation tank, and the fluid outlets of the plurality of extraction separation units are respectively communicated with the outlet of the gaseous fluid storage tank;
and the second heat exchange medium circulation loops are respectively formed between the first heat exchange medium storage device and the second heat exchange devices corresponding to the extraction separation units.
In some embodiments of the invention, the fractionation purification subsystem includes at least one distiller and at least one condensing chamber, the distiller being disposed in correspondence with the condensing chamber; the material outlet of the first material storage tank is communicated with the material inlet of the distiller, the vaporization part is positioned on the distiller, and the material inlet of the distiller is arranged on the vaporization part; the vacuum outlet of the distiller is communicated with the vacuum inlet corresponding to the condensing chamber, and the vacuum outlet of the condensing chamber is connected with a vacuum pump; the extract outlet of the distiller and the extract outlet of the condensing chamber are respectively connected with an extract storage tank, and the material outlet of the distiller is connected with a second material storage tank; the condensing part comprises a first condensing part and a second condensing part, the first condensing part is positioned on the distiller, and an extract outlet of the distiller is arranged on the first condensing part; the second condensing part is positioned on the condensing chamber, and an extract outlet of the condensing chamber is arranged on the second condensing part;
The first heat supply unit comprises a fourth heat exchange device and a second heat exchange medium storage device, a third heat exchange medium circulation loop is formed between the fourth heat exchange device and the second heat exchange medium storage device, and a fourth heat exchange medium circulation loop is formed between the second heat exchange medium storage device and the vaporization part;
the second cooling unit comprises a first cooling subunit and a second cooling subunit which are connected in parallel; the inlets of the first cooling subunit and the second cooling subunit parallel passages are communicated with the second heat supply unit, and the outlets of the first cooling subunit and the second cooling subunit parallel passages are communicated with the compression unit; the first cooling subunit comprises a second throttling expansion device and a second carbon dioxide storage tank which are connected in series along the flowing direction of carbon dioxide, and a second carbon dioxide circulation loop is formed between the second carbon dioxide storage tank and the first condensing part; the second cooling subunit comprises a third throttling expansion device and a third carbon dioxide storage tank which are connected in series, and a third carbon dioxide circulation loop is formed between the third carbon dioxide storage tank and the second condensation part.
In some embodiments of the invention, the fractionation purification subsystem includes a plurality of the distillers and a plurality of the condensing chambers;
The plurality of distillers are connected in series step by step, the material outlet of the first material storage tank is communicated with the material inlet of the distiller positioned at the first stage, the material outlet of each distiller is respectively connected with the second material storage tank, the material outlet of the second material storage tank positioned at the upper stage is communicated with the material inlet of the distiller positioned at the lower stage, and an emptying branch is further arranged on a connecting pipeline between the material outlet of the second material storage tank and the material inlet of the distiller positioned at the lower stage;
the second heat exchange medium storage device and the vaporization parts of the plurality of distillers respectively form the fourth heat exchange medium circulation loop; the second carbon dioxide circulation loops are respectively formed between the second carbon dioxide storage tank and the first condensation parts of the plurality of distillers; and the third carbon dioxide circulating loops are respectively formed between the third carbon dioxide storage tank and the second condensing parts of the condensing chambers.
In some embodiments of the invention, the processing system includes a first filter and a second filter; the first filter is arranged on a pipeline between the gaseous fluid storage tank and the first heat exchange device, and a fluid outlet of the extraction separation unit and a fluid outlet of the gaseous fluid separation tank are communicated with the pipeline between the first filter and the gaseous fluid storage tank; the gaseous fluid outlet of the gas-liquid separation tank is connected to a pipeline between the first heat exchange device and the first filter; the second filter is arranged on a pipeline between the liquid fluid storage tank and the extraction separation unit; a booster pump is further arranged on a pipeline between the liquid fluid storage tank and the second filter;
The processing system further includes an entrainer subsystem including an entrainer reservoir and an entrainer delivery pump; the outlet of the entrainer storage tank is connected to a pipeline between the booster pump and the second filter through an entrainer delivery pipeline, and the entrainer delivery pump is arranged on the entrainer delivery pipeline.
A second aspect of the present invention proposes a control method of a processing system for extracting plant active ingredients by supercritical fluid, which is implemented by the processing system proposed by the first aspect of the present invention; the control method comprises the following steps:
the method comprises the steps of controlling a first heat exchange medium circulation loop, a third heat exchange medium circulation loop and a first carbon dioxide circulation loop of the carbon dioxide cold and hot combined supply subsystem to start;
controlling the supercritical fluid extraction subsystem to start to operate according to the condition that the temperature of a first heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem reaches a first temperature condition and the temperature of a first carbon dioxide storage tank reaches a second temperature condition;
and controlling the fractionation and purification subsystem to start operation.
According to the control method, reasonable control logic is arranged on the processing system to realize efficient and high-purity extraction of plant active ingredients and low-energy-consumption operation of the processing system.
In addition, the control method according to the present invention may further have the following additional technical features:
in some embodiments of the invention, in the step of controlling the start-up operation of the supercritical fluid extraction subsystem, the method comprises:
controlling a material to be extracted to enter an extraction kettle of the supercritical fluid extraction subsystem, and controlling a passage between a gaseous fluid storage tank and a liquid fluid storage tank of the supercritical fluid extraction subsystem to be communicated;
according to the condition that the pressure of the liquid fluid storage tank reaches a first pressure, controlling a second heat exchange medium circulation loop of the carbon dioxide cold and hot combined supply subsystem to start, and controlling a passage between the gaseous fluid storage tank and the extraction kettle to be communicated;
controlling the flow of carbon dioxide between the gaseous fluid storage tank and the extraction kettle, controlling the passage conduction between the extraction kettle and the separation kettle of the supercritical fluid extraction subsystem according to the condition that the pressure of the extraction kettle reaches a second pressure, and maintaining the pressure of the extraction kettle at the second pressure;
controlling the passage conduction between the fluid outlet of the separation kettle and the fluid outlet of the gaseous fluid storage tank according to the condition that the pressure of the separation kettle reaches the third pressure, and maintaining the pressure of the extraction kettle under the third pressure condition;
According to the extraction time of the extraction kettle reaching the set extraction time, controlling the passages between the liquid fluid storage tank and the extraction kettle, between the extraction kettle and the separation kettle and between the separation kettle and the gaseous fluid storage tank to be respectively disconnected, and controlling the material outlet of the separation kettle to be communicated with the passage between the gaseous fluid separation tank of the supercritical fluid extraction subsystem;
and controlling the disconnection of a passage between a material outlet of the separation kettle and the gaseous fluid separation tank according to the emptying of the extract in the separation kettle, controlling the connection of an emptying pipeline of the supercritical fluid extraction subsystem, and controlling the closing of the emptying pipeline according to the condition that the pressure of the extraction kettle reaches the fourth pressure.
In some embodiments of the present invention, the temperature of the first heat exchange medium storage device is T1, the fluid outlet temperature of the second heat exchange device of the carbon dioxide cold and hot combined supply subsystem corresponding to the first heat exchange medium storage device is T01, and the first temperature condition is: t1 is more than or equal to T01+ and is at a first set temperature;
the temperature of the first carbon dioxide storage tank is T2, the fluid outlet temperature of the first heat exchange device of the carbon dioxide cold and hot combined supply subsystem is T02, and the second temperature condition is as follows: t2 is more than or equal to T02-second set temperature.
In some embodiments of the invention, the step of controlling the start-up operation of the fractionation purification subsystem comprises:
controlling a fourth heat exchange medium circulation loop of the carbon dioxide cold and hot combined supply subsystem to start according to the condition that the temperature of a second heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem reaches a third temperature;
controlling a second carbon dioxide circulation loop and a third carbon dioxide circulation loop of the carbon dioxide cold and hot combined supply subsystem to start according to the condition that the temperature of a second carbon dioxide storage tank of the carbon dioxide cold and hot combined supply subsystem reaches a fourth temperature condition and the temperature of a third carbon dioxide storage tank reaches a fifth temperature condition;
controlling a vacuum pump of the fractionation and purification subsystem to start, and controlling a first material storage tank of the supercritical fluid extraction subsystem to convey a first material to a distiller of the fractionation and purification subsystem according to a fifth pressure condition reached by the pressure of the distiller;
and controlling the communication between the distiller and a second material storage tank of the fractional distillation and purification subsystem according to the distillation time of the distiller reaching the set distillation time.
In some embodiments of the present invention, the temperature of the second heat exchange medium storage device is T3, the distillation temperature of the distiller is T03, and the third temperature condition is: t3 is more than or equal to T03+ and is at a third set temperature;
The temperature of the second carbon dioxide storage tank is T4, the condensation temperature of the distiller is T04, and the fourth temperature condition is: t4 is more than or equal to T04+ and is at a fourth set temperature;
the temperature of the third carbon dioxide storage tank is T5, the temperature of the condensing chamber is T05, and the fifth temperature condition is: t5 is greater than or equal to T05 and is at a fifth set temperature.
In some embodiments of the invention, prior to the step of controlling the start-up of the fractionation purification subsystem, the control method further comprises: controlling the entrainer subsystem start-up of the processing system.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
fig. 1 schematically illustrates a system block diagram of a processing system according to an embodiment of the present invention.
Fig. 2 schematically shows a system configuration diagram of a processing system according to an embodiment of the present invention.
Fig. 3 schematically shows a control flow diagram of a processing system according to another embodiment of the invention.
Fig. 4 schematically shows a control flow diagram of a processing system according to another embodiment of the invention.
Fig. 5 schematically shows a control flow diagram of a processing system according to another embodiment of the invention.
Fig. 6 schematically illustrates a control flow diagram of a processing system in accordance with one embodiment of the present invention.
Reference numerals illustrate:
10a, a supercritical fluid extraction subsystem; 101a, a first fluid branch; 102a, a second fluid branch; 20a, a fractional distillation purification subsystem; 201a, a vaporization part; 202a, a condensing part; 1a, a first condensing part; 2a, a second condensing part; 30a, a carbon dioxide cold and hot combined supply subsystem; 301a, a compression unit; 302a, a first heating unit; 303a, a second heating unit; 304a, a first cooling unit; 305a, a second cooling unit; 40a, an entrainer subsystem; 1b, a first heat exchange medium circulation loop; 2b, a second heat exchange medium circulation loop; 3b, a third heat exchange medium circulation loop; 4b, a fourth heat exchange medium circulation loop; 1c, a first carbon dioxide circulation loop; 2c, a second carbon dioxide circulation loop; 3c, a third carbon dioxide circulation loop;
1. a gaseous fluid reservoir; 2. a gas-liquid separation tank; 3. a liquid fluid storage tank; 4. a booster pump; 501-534, first electromagnetic valve-thirty-fourth electromagnetic valve; 601. a first filter; 602. a second filter; 701 to 711, first heat exchanger to eleventh heat exchanger; 801. a first evacuation line; 802. a second evacuation line; 803. an evacuation branch; 901. a first flowmeter; 902. a second flowmeter; 903. an entrainer flow meter; 101. a first extraction tank; 102. a second extraction kettle; 111-114, a first separation kettle-a fourth separation kettle; 12. a storage tank for the extract to be extracted; 13. an entrainer storage tank; 141-143, a first carbon dioxide storage tank-a third carbon dioxide storage tank; 15. an entrainer delivery pump; 16. a gaseous fluid separation tank; 171. a first material storage tank; 172. a second material storage tank; 173. a residue storage tank; 181. a first distiller; 182. a second distiller; 191-194, a first extract storage tank-a fourth extract storage tank; 201. a first condensing chamber; 202. a second condensing chamber; 211. a first vacuum pump; 212. a second vacuum pump; 221. a first compressor; 222. a second compressor; 231-233, first-third throttle expansion devices; 241 to 243, and first to third carbon dioxide transfer pumps; 251 to 258, a first water delivery pump to an eighth water delivery pump; 261. a first material transfer pump; 262. a second material transfer pump; 271-274, first heat exchange medium storage tank-fourth heat exchange medium storage tank.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It is to be understood that the terminology used herein is for the purpose of describing particular example embodiments only, and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprises," "comprising," "includes," "including," and "having" are inclusive and therefore specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof. The method steps, processes, and operations described herein are not to be construed as necessarily requiring their performance in the particular order described or illustrated, unless an order of performance is explicitly stated. It should also be appreciated that additional or alternative steps may be used.
Although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms may be only used to distinguish one element, component, region, layer or section from another region, layer or section. Terms such as "first," "second," and other numerical terms when used herein do not imply a sequence or order unless clearly indicated by the context. Thus, a first element, component, region, layer or section discussed below could be termed a second element, component, region, layer or section without departing from the teachings of the example embodiments.
For ease of description, spatially relative terms, such as "inner," "outer," "lower," "below," "upper," "above," and the like, may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. Such spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" or "over" the other elements or features. Thus, the example term "below … …" may include both upper and lower orientations. The device may be otherwise oriented (rotated 90 degrees or in other directions) and the spatial relative relationship descriptors used herein interpreted accordingly.
As shown in fig. 1 and 2, according to an embodiment of the present invention, a processing system for extracting plant active ingredients, such as essence, essential oil and waxy active, by supercritical fluid is provided, and the processing system of this example is used for extracting plant active ingredients, such as aromatic plants. Referring to fig. 1, the processing system of the present embodiment includes a supercritical fluid extraction subsystem 10a, a fractionation purification subsystem 20a, and a carbon dioxide cold and hot combined supply subsystem 30a. The supercritical fluid adopts carbon dioxide because of its high density and high capability of dissolving the active ingredient. The supercritical fluid extraction subsystem 10a is used for separating a first material containing an active ingredient from a material to be extracted by using supercritical carbon dioxide, for example, the supercritical fluid extraction subsystem 10a combines an extraction process and a separation process to separate the first material containing the active ingredient from the material to be extracted. Along the flow direction of the carbon dioxide, the supercritical fluid extraction subsystem 10a comprises a first fluid branch 101a and a second fluid branch 102a connected in series, wherein the first fluid branch 101a is used for converting gaseous carbon dioxide into liquid carbon dioxide, and the second fluid branch 102a is used for dissolving a first material containing active ingredients in a material to be extracted by utilizing supercritical carbon dioxide so as to extract and separate the first material. The second fluid branch 102a may be one or more, and when a plurality of second fluid branches 102a are provided, the plurality of second fluid branches 102a are connected in parallel. Illustratively, referring to FIG. 2, there are two second fluid branches 102a, with the inlets of the parallel passages of the two second fluid branches 102a communicating with the outlet of the first fluid branch 101 a. The fractionation purification subsystem 20a is in series with a second fluid leg 102a in the supercritical fluid extraction subsystem 10a, with the material outlet of the second fluid leg 102a being in communication with the material inlet of the fractionation purification subsystem 20 a. Referring to fig. 2, the material outlets of the parallel paths of the two second fluid branches 102a are each in communication with the material inlet of the fractionation purification subsystem 20 a. The fractionation purification subsystem 20a is used to purify the active ingredient in the separated first material, for example, the separation purification subsystem uses a distillation process to purify the active ingredient in the first material. The fractionation and purification subsystem 20a includes a vaporizing portion 201a and a condensing portion 202a, and the active ingredient in the first material entering the fractionation and purification subsystem 20a is vaporized in the vaporizing portion 201a, and the vaporized active ingredient is condensed in the condensing portion 202a, thereby separating the active ingredient from the first material.
The carbon dioxide combined heat and cold supply subsystem 30a includes a compression unit 301a, a first heat supply unit 302a, a second heat supply unit 303a, a first cooling unit 304a, and a second cooling unit 305a. Along the flow direction of the carbon dioxide, the compression unit 301a, the first heat supply unit 302a and the second heat supply unit 303a are sequentially connected in series, the first cooling unit 304a and the second cooling unit 305a are connected in parallel, and the inlet of the parallel passage of the first cooling unit 304a and the second cooling unit 305a is communicated with the second heat supply unit 303a, and the outlet of the parallel passage of the first cooling unit 304a and the second cooling unit 305a is communicated with the compression unit 301 a. The compression unit 301a includes at least one compressor, and illustratively, as shown in fig. 2, the compression unit 301a includes a first compressor 221 and a second compressor 222 connected in parallel. The first cooling unit 304a performs heat exchange with the first fluid branch 101a to cool and condense the gaseous carbon dioxide in the first fluid branch 101a into liquid carbon dioxide. The second heat supply unit 303a exchanges heat with the second fluid branch 102a, and the supercritical carbon dioxide in the second fluid branch 102a is heated to reach a preset extraction temperature or separation temperature. The first heat supply unit 302a exchanges heat with the vaporizing portion 201a to heat up and vaporize the active ingredient in the first material entering the vaporizing portion 201 a. The second cooling unit 305a exchanges heat with the condensing part 202a to condense the vaporized active ingredient, thereby separating the active ingredient from the first material.
The processing system of the embodiment is provided with the carbon dioxide cold and hot combined supply subsystem 30a so that the supercritical fluid extraction subsystem 10a and the fractionation purification subsystem 20a work at a proper temperature, and other unwanted compounds in plants are prevented from being extracted, so that the purity of active ingredients is improved. Meanwhile, heat supply and refrigeration respectively generate energy consumption in the traditional supercritical fluid extraction process, and the carbon dioxide cold and heat combined supply subsystem 30a of the embodiment can realize heat supply and refrigeration at the same energy consumption, so that the energy consumption of a processing system is reduced.
According to an embodiment of the present invention, as shown in fig. 2, the supercritical fluid extraction subsystem 10a includes a to-be-extracted storage tank 12, a gaseous fluid storage tank 1, a first heat exchange device, a gas-liquid separation tank 2, a liquid fluid storage tank 3, an extraction separation unit, a gaseous fluid separation tank 16, and a first material storage tank 171, the first heat exchange device corresponding to the first heat exchanger 701 in fig. 2.
Along the flow direction of carbon dioxide, the gaseous fluid storage tank 1, the first heat exchanger 701, the gas-liquid separation tank 2 and the liquid fluid storage tank 3 are sequentially connected in series on the first fluid branch 101a, gaseous carbon dioxide is stored in the gaseous fluid storage tank 1, the first heat exchanger 701 and the first cooling unit 304a are correspondingly arranged, and the first heat exchanger 701 and the first cooling unit 304a perform heat exchange so that gaseous carbon dioxide entering the first heat exchanger 701 is cooled and condensed to form liquid carbon dioxide. The gas-liquid separation tank 2 is used for separating the gaseous carbon dioxide which flows out of the first heat exchanger 701 and is not condensed yet from the liquid carbon dioxide, the gaseous fluid outlet of the gas-liquid separation tank 2 is communicated with the fluid inlet of the first heat exchanger 701, the separated gaseous carbon dioxide flows into the first heat exchanger 701 again, and the separated liquid carbon dioxide enters the liquid fluid storage tank 3.
The extraction separation unit is arranged on the second fluid branch 102a, and is used for separating the first material containing the effective components from the to-be-extracted matters entering the extraction separation unit by utilizing supercritical carbon dioxide. The storage tank 12 for the materials to be extracted is used for storing the materials to be extracted, and the storage tank 12 for the materials to be extracted is communicated with a material inlet of the extraction separation unit. The material outlet of the extraction separation unit is in communication with a gaseous fluid separation tank 16, the gaseous fluid separation tank 16 being adapted to separate gaseous carbon dioxide and a first material exiting the material outlet of the extraction separation unit. The material outlet of the gaseous fluid separation tank 16 communicates with the first material storage tank 171, and the separated first material flows into the first material storage tank 171 for storage. The fluid outlet of the extraction separation unit and the fluid outlet of the gaseous fluid separation tank 16 are both communicated with the outlet of the gaseous fluid storage tank 1, and the gaseous carbon dioxide discharged from the fluid outlet of the extraction separation unit and the gaseous carbon dioxide separated by the gaseous fluid separation tank 16 flow back to the fluid outlet of the gaseous fluid storage tank 1 again, and the gaseous carbon dioxide flowing out of the gaseous fluid storage tank 1 is converged and then enters the first heat exchanger 701 again.
The first cooling unit 304a includes a first throttling expansion device 231 and a first carbon dioxide storage tank 141 connected in series in the flow direction of carbon dioxide, the first throttling expansion device 231 is communicated with the second heating unit 303a, and a fluid outlet of the first carbon dioxide storage tank 141 is communicated with the compression unit 301 a. The first throttling expansion device 231 is used for throttling and depressurizing the liquid carbon dioxide flowing into the first throttling expansion device to generate low-temperature low-pressure two-phase carbon dioxide, the low-temperature low-pressure liquid carbon dioxide flows into the first carbon dioxide storage tank 141 to be buffered, a first carbon dioxide circulation loop 1c is formed between the first carbon dioxide storage tank 141 and the first heat exchange device to absorb heat of the gaseous carbon dioxide entering the first heat exchange device, and the gaseous carbon dioxide in the first heat exchange device is condensed to form liquid carbon dioxide. The second heat supply unit 303a performs heat exchange with the extraction separation unit, so that the extraction separation unit can separate the first material from the material to be extracted at a proper temperature, thereby avoiding the extraction of unwanted compounds at an excessive temperature and ensuring the purity of the final product.
According to an embodiment of the present invention, as shown in fig. 2, the extraction separation unit includes an extraction tank, at least one separation tank, and a plurality of second heat exchange devices, which are connected in series with the extraction tank along a flow direction of carbon dioxide, and the plurality of second heat exchange devices are respectively disposed at the extraction tank, and at fluid inlets of the separation tank. Referring to fig. 2, the processing system includes two extraction separation units connected in parallel, the extraction kettles include a first extraction kettle 101 and a second extraction kettle 102, each extraction separation unit includes two separation kettles connected in series, wherein the first extraction kettle 101, the first separation kettle 111 and the second separation kettle 112 are connected in series, the second extraction kettle 102, the third separation kettle 113 and the fourth separation kettle 114 are connected in series, the plurality of second heat exchangers are a second heat exchanger 702 to a seventh heat exchanger 707, and the second heat exchanger 702 to the seventh heat exchanger 707 are respectively arranged at fluid inlets of the first extraction kettle 101, the second extraction kettle 102, the first separation kettle 111 and the fourth separation kettle 114. The second heat supply unit 303a performs heat exchange with the plurality of second heat exchange devices, referring to fig. 2, the second heat supply unit 303a performs heat exchange with the second heat exchanger 702 to the seventh heat exchanger 707, respectively, to heat the carbon dioxide entering the plurality of second heat exchange devices, thereby regulating and controlling the temperature of the carbon dioxide entering the extraction kettle and the separation kettle, so as to enable the carbon dioxide entering the extraction kettle to reach an extraction temperature condition capable of better dissolving the first material, and enable the temperature of the supercritical carbon dioxide entering the separation kettle to reach an optimal separation temperature condition capable of enabling the supercritical carbon dioxide to be changed into a gaseous state so as to separate the first material.
The material outlet of the to-be-extracted material storage tank 12 is communicated with the material inlet of the extraction kettle, supercritical carbon dioxide flowing out of the first fluid branch 101a enters the extraction kettle, and referring to fig. 2, the material outlet of the to-be-extracted material storage tank 12 respectively enters the material inlets of the first extraction kettle 101 and the second extraction kettle 102, and supercritical carbon dioxide flowing out of the first fluid branch 101a respectively flows into the fluid inlets of the first extraction kettle 101 and the second extraction kettle 102. According to the embodiment, the characteristic that the supercritical carbon dioxide dissolves the first material is utilized, so that the extraction of the first material in the material to be extracted is realized, meanwhile, the supercritical carbon dioxide is changed into the gaseous state by adjusting the temperature of the carbon dioxide entering the separating valve through the second heat supply unit 303a, and the separation of the carbon dioxide and the first material is realized.
Referring to fig. 2, a mixture containing supercritical carbon dioxide and a first material enters a separation kettle through an extraction kettle, a material outlet of the separation kettle is communicated with a gaseous fluid separation tank 16, the first material separated by the separation kettle carries a small amount of gaseous carbon dioxide into the gaseous fluid separation tank 16, and the gaseous fluid separation tank 16 separates the gaseous carbon dioxide from the first material. The fluid outlet of the separation kettle is communicated with the outlet of the gaseous fluid storage tank 1, and the gaseous carbon dioxide separated by the separation kettle and the gaseous carbon dioxide separated by the gaseous fluid storage tank 1 are converged and then re-enter the first heat exchanger 701. The extraction separation unit of this embodiment may be provided with one separation tank, or may be provided with a plurality of separation tanks, and when a plurality of separation tanks are provided, the plurality of separation tanks are connected in series, and the material outlet of each separation tank is communicated with the gaseous fluid separation tank 16, and the fluid outlet of the separation tank located at the last stage is communicated with the outlet of the gaseous fluid storage tank 1. The bottom of the extraction kettle is provided with an emptying pipeline which is used for emptying the carbon dioxide in the extraction kettle. Referring to fig. 2, a first evacuation line 801 is provided at the bottom of the first extraction tank 101, and a second evacuation line 802 is provided at the bottom of the second extraction tank 102.
The second heat supply unit 303a includes a plurality of third heat exchange devices and a plurality of first heat exchange medium storage devices, the plurality of third heat exchange devices being connected in series. Referring to fig. 2, the plurality of third heat exchange devices are ninth to eleventh heat exchangers 709 to 711 connected in series in the flow direction of carbon dioxide, and the plurality of first heat exchange medium storage devices are first to third heat exchange medium storage tanks 271 to 273. The third heat exchange device is arranged corresponding to the first heat exchange medium storage device, and the first heat exchange medium storage device is arranged corresponding to the second heat exchange device. Referring to fig. 2, the ninth heat exchanger 709 corresponds to a first heat exchange medium storage tank 271, and the first heat exchange medium storage tank 271 corresponds to a fourth heat exchanger 704; the tenth heat exchanger 710 corresponds to the second heat exchange medium storage tank 272, and the second heat exchange medium storage tank 272 corresponds to the third heat exchanger 703; the eleventh heat exchanger 711 corresponds to the third heat exchange medium storage tank 273, and the third heat exchange medium storage tank 273 corresponds to the second heat exchanger 702. A first heat exchange medium circulation loop 1b is formed between the third heat exchange device and the corresponding first heat exchange medium storage device, the third heat exchange device transmits heat to the heat exchange medium of the first heat exchange medium storage device through the first heat exchange medium circulation loop 1b, and the heat exchange medium can be water or other heat carriers. Referring to fig. 2, a first heat exchange medium circulation circuit 1b is formed between the ninth heat exchanger 709 and the first heat exchange medium storage tank 271, between the tenth heat exchanger 710 and the second heat exchange medium storage tank 272, and between the eleventh heat exchanger 711 and the third heat exchange medium storage tank 273, respectively. A second heat exchange medium circulation loop 2b is formed between the first heat exchange medium storage device and the corresponding second heat exchange device, so that heat is transferred to the carbon dioxide in the second heat exchange device through the second heat exchange medium circulation loop 2b, and the carbon dioxide flowing through the second heat exchange device is heated, so that the temperature of the carbon dioxide reaches a proper extraction temperature or separation temperature. Referring to fig. 2, a second heat exchange medium circulation loop 2b is formed between the first heat exchange medium storage tank 271 and the fourth heat exchanger 704, between the second heat exchange medium storage tank 272 and the third heat exchanger 703, and between the third heat exchange medium storage tank 273 and the second heat exchanger 702, respectively.
According to an embodiment of the present invention, as shown in fig. 2, the processing system includes a plurality of extraction separation units, the plurality of extraction separation units are connected in parallel, a material outlet of the to-be-extracted material storage tank 12 is respectively communicated with material inlets of the plurality of extraction separation units, and fluid outlets of the plurality of extraction separation units are respectively communicated with an outlet of the gaseous fluid storage tank 1. And second heat exchange medium circulation loops 2b are respectively formed between the first heat exchange medium storage devices and the corresponding second heat exchange devices of the extraction separation units so as to adjust the temperatures of the extraction tanks and the separation tanks, in which the carbon dioxide enters the extraction separation units respectively, to reach proper temperatures. Referring to fig. 2, a first heat exchange medium storage tank 271 corresponds to a fourth heat exchanger 704 and a seventh heat exchanger 707, a second heat exchange medium storage tank 272 corresponds to a third heat exchanger 703 and a sixth heat exchanger 706, and a third heat exchange medium storage tank 273 corresponds to a second heat exchanger 702 and a fifth heat exchanger 705. A second heat exchange medium circulation loop 2b is formed between the first heat exchange medium storage tank 271 and the fourth heat exchanger 704 and the seventh heat exchanger 707, between the second heat exchange medium storage tank 272 and the third heat exchanger 703 and the sixth heat exchanger 706, and between the third heat exchange medium storage tank 273 and the second heat exchanger 702 and the fifth heat exchanger 705, respectively. The embodiment can control the plurality of extraction separation units to operate sequentially in different time periods in a day so as to realize continuous and uninterrupted operation of the supercritical fluid extraction subsystem 10 a; meanwhile, part of extraction separation units can be controlled to operate, and other extraction separation units are used as spare parts to ensure the reliability of the supercritical fluid extraction subsystem 10 a; in addition, all extraction separation units can be controlled to operate simultaneously, so that the extraction yield of the active ingredients in the plants can be improved.
According to an embodiment of the present invention, as shown in fig. 2, the fractionation purification subsystem 20a includes at least one distiller and at least one condensing chamber, the distiller being disposed in correspondence with the condensing chamber. The material outlet of the first material storage tank 171 is communicated with the material inlet of the distiller, and the distiller distills the first material to extract the effective components in the first material. As shown in fig. 2, the fractionation purification subsystem 20a includes two distillers, namely, a first distiller 181 and a second distiller 182, where the first distiller 181 is provided with a first condensing chamber 201 and the second distiller 182 is provided with a second condensing chamber 202. The vaporization part 201a is located on the distiller, the material inlet of the distiller is arranged on the vaporization part 201a, and after the first material enters the distiller, the effective components in the first material are vaporized in the vaporization part 201 a. The vacuum outlet of the distiller is communicated with the vacuum inlet of the corresponding condensing chamber, a small amount of active ingredients discharged into the condensing chamber from the vacuum outlet are further condensed in the condensing chamber, the vacuum outlet of the condensing chamber is connected with a vacuum pump, referring to fig. 2, the first vacuum pump 211 is communicated with the vacuum outlet of the first condensing chamber 201, and the second vacuum pump 212 is communicated with the vacuum outlet of the second condensing chamber 202. The vacuum pump is used for vacuumizing the distiller and the condensing chamber respectively so as to reduce the boiling points of the active ingredients in the distiller and the condensing chamber, so that the active ingredients are vaporized, the residual ingredients in the first material are not vaporized, and the purity of the active ingredients is ensured. The condensing unit 202a includes a first condensing unit 1a and a second condensing unit 2a, the first condensing unit 1a is located on the distiller, an extract outlet of the distiller is disposed on the first condensing unit 1a, and the first condensing unit 1a condenses the vaporized active ingredient in the distiller to form a liquid active ingredient. The second condensation part 2a is located on the condensation chamber, the extract outlet of the condensation chamber is arranged on the second condensation part 2a, and the second condensation part 2a condenses the vaporized active ingredient entering the condensation chamber to form liquid active ingredient. The extract outlet of the distiller and the extract outlet of the condensing chamber are respectively connected to an extract storage tank, referring to fig. 2, the extract outlet of the first distiller 181 is connected to a first extract storage tank 191, the extract outlet of the first condensing chamber 201 is connected to a second extract storage tank 192, the extract outlet of the second distiller 182 is connected to a third extract storage tank 193, the extract outlet of the second condensing chamber 202 is connected to a fourth extract storage tank 194 to collect liquid active ingredients flowing out of the distiller and the condensing chamber, respectively, and the material outlet of the distiller is connected to a second material storage tank 172.
The first heat supply unit 302a includes a fourth heat exchange device and a second heat exchange medium storage device, a third heat exchange medium circulation loop 3b is formed between the fourth heat exchange device and the second heat exchange medium storage device, the fourth heat exchange device is communicated with the air outlet of the compression unit 301a, high-temperature and high-pressure gaseous carbon dioxide enters the fourth heat exchange device, and the gaseous carbon dioxide transfers part of heat into the heat exchange medium through the third heat exchange medium circulation loop 3 b. A fourth heat exchange medium circulation loop 4b is formed between the second heat exchange medium storage device and the vaporizing part 201a, and the heat exchange medium transfers heat to the vaporizing part 201a through the fourth heat exchange medium circulation loop 4b, so that the effective components in the first material in the vaporizing part 201a are vaporized, and the effective components are separated from other components in the first material. Referring to fig. 2, the fourth heat exchange device is an eighth heat exchanger 708, the second heat exchange medium storage device is a fourth heat exchange medium storage tank 274, a third heat exchange medium circulation loop 3b is formed between the eighth heat exchanger 708 and the fourth heat exchange medium storage tank 274, and a fourth heat exchange medium circulation loop 4b is formed between the fourth heat exchange medium storage tank 274 and the first distiller 181 and the second distiller 182, respectively.
The second cooling unit 305a includes a first cooling subunit and a second cooling subunit connected in parallel, an inlet of a parallel path of the first cooling subunit and the second cooling subunit is communicated with the second heat supply unit 303a, an outlet of the parallel path of the first cooling subunit and the second cooling subunit is communicated with the compression unit 301a, and the carbon dioxide flowing out of the fourth heat exchange device transfers the residual heat to the heat exchange medium through the first heat exchange medium circulation loop 1b of the second heat supply unit 303 a. The carbon dioxide flowing out of the second heat supply unit 303a enters the first cooling unit 304a and the second cooling unit 305a respectively, and the carbon dioxide entering the second cooling unit 305a continues to enter the first cooling subunit and the second cooling subunit in two branches. Along the carbon dioxide flow direction, the first cooling subunit includes a second throttling expansion device 232 and a second carbon dioxide storage tank 142 connected in series, and a second carbon dioxide circulation loop 2c is formed between the second carbon dioxide storage tank 142 and the first condensation portion 1 a. The carbon dioxide flows into the second throttling expansion device 232 and is throttled and depressurized by the second throttling expansion device 232 to become a low-temperature and low-pressure carbon dioxide two-phase flow, wherein the low-temperature and low-pressure liquid carbon dioxide cools the first condensation part 1a by the second carbon dioxide circulation loop 2c, so that the vaporized active ingredients are condensed into a liquid state. The second cooling subunit includes a third throttling expansion device 233 and a third carbon dioxide storage tank 143 connected in series, a third carbon dioxide circulation loop 3c is formed between the third carbon dioxide storage tank 143 and the second condensation portion 2a, high-temperature and high-pressure carbon dioxide flows into the third throttling expansion device 233 and then throttled and depressurized by the third throttling expansion device 233 to become a low-temperature and low-pressure carbon dioxide two-phase flow, and low-temperature and low-pressure liquid carbon dioxide cools the second condensation portion 2a through the third carbon dioxide circulation loop 3c, so that the vaporized active ingredients are condensed into a liquid state. The gaseous carbon dioxide discharged from the second and third carbon dioxide tanks 142 and 143 finally flows back to the suction port of the compression unit 301a to enter the next combined cooling and heating cycle of carbon dioxide.
According to an embodiment of the present invention, as shown in fig. 2, the fractionation purification subsystem 20a includes a plurality of distillers and a plurality of condensing chambers, the plurality of distillers being disposed corresponding to the plurality of condensing chambers. The plurality of distillers are serially connected step by step, the material outlet of the first material storage tank 171 is communicated with the material inlet of the distiller positioned at the first stage, the material outlet of each distiller is respectively connected with the second material storage tank 172, and the material outlet of the second material storage tank 172 positioned at the distiller positioned at the previous stage is communicated with the material inlet of the distiller positioned at the next stage. The present embodiment further achieves extraction purity of the effective substance by providing a plurality of distillers and a plurality of condensing chambers. An emptying branch 803 is further arranged on a connecting pipeline between the material outlet of the second material storage tank 172 and the material inlet of the distiller positioned at the next stage, and the emptying branch 803 is used for emptying residual materials in the second material storage tank 172. Referring to fig. 2, the material outlets of the first distiller 181 and the second distiller 182 are respectively connected to the second material storage tank 172, the material outlet of the second material storage tank 172 corresponding to the first distiller 181 is communicated with the material inlet of the second distiller 182, and an evacuation branch 803 is provided on a communicating pipe between the second material storage tank 172 and the second distiller 182. Fourth heat exchange medium circulation circuits 4b are respectively formed between the second heat exchange medium storage device and the plurality of distillers to heat the vaporization parts 201a of the plurality of distillers, respectively. The second carbon dioxide circulation loop 2c is formed between the second carbon dioxide storage tank 142 and the plurality of distillers, respectively, to cool the first condensing units 1a of the plurality of distillers, respectively. A third carbon dioxide circulation loop 3c is formed between the third carbon dioxide tank 143 and the plurality of condensation chambers, respectively, to cool the second condensation parts 2a of the plurality of condensation chambers, respectively. Referring to fig. 2, a fourth heat exchange medium circulation loop 4b is formed between the fourth heat exchange medium storage tank 274 and the vaporizing portion 201a of the first distiller 181 and the vaporizing portion 201a of the second distiller 182, respectively. The second carbon dioxide storage tank 142 forms a second carbon dioxide circulation loop 2c with the first condensing portion 1a of the first distiller 181 and the first condensing portion 1a of the second distiller 182, respectively. A third carbon dioxide circulation loop 3c is formed between the third carbon dioxide tank 143 and the second condensation part 2a of the first condensation chamber 201 and the second condensation part 2a of the second condensation chamber 202, respectively.
According to an embodiment of the present invention, as shown in fig. 2, the processing system of the present embodiment includes a first filter 601 and a second filter 602, the first filter 601 being disposed on a pipe between the gaseous fluid reservoir 1 and the first heat exchanger 701. The fluid outlet of the extraction separation unit and the fluid outlet of the gaseous fluid separation tank 16 are both communicated with a pipeline between the first filter 601 and the gaseous fluid storage tank 1, and the gaseous fluid outlet of the gas-liquid separation tank 2 is positioned on the pipeline between the first heat exchanger 701 and the first filter 601 so as to filter the gaseous carbon dioxide entering the first heat exchanger 701. A second filter 602 is provided on the conduit between the liquid fluid reservoir 3 and the extraction separation unit to filter the carbon dioxide entering the extraction separation unit. A booster pump 4 is further arranged on a pipeline between the liquid fluid storage tank 3 and the second filter 602, the booster pump 4 provides pressure for carbon dioxide to enter the extraction separation unit, and the liquid carbon dioxide is converted into supercritical carbon dioxide through the booster pump 4.
According to an embodiment of the present invention, as shown in fig. 2, the processing system of the present embodiment further comprises an entrainer subsystem 40a, the entrainer subsystem 40a comprising an entrainer reservoir 13 and an entrainer delivery pump 15, the outlet of the entrainer reservoir 13 being connected to the conduit between the booster pump 4 and the second filter 602 by an entrainer delivery conduit, the entrainer delivery pump 15 being arranged on the entrainer delivery conduit. The entrainer may alter the solubility of the solute and the solubility of carbon dioxide. The entrainer, such as water, methanol, ethanol, acetone, propane, etc., the entrainer subsystem 40a may be turned on or off as determined by actual demand.
The processing system of this embodiment will be described in detail below with reference to the specific example of fig. 2, where the supercritical fluid extraction subsystem 10a includes two parallel extraction separation units, each of which is provided with two separation tanks in series, and the fractionation and purification subsystem 20a includes two distillation units in series stage by stage, and each distillation unit is provided with a condensation chamber correspondingly. In the processing system of the present embodiment, the heat exchange medium is water, the first heat exchange device is a first heat exchanger 701, the plurality of second heat exchange devices is a second heat exchanger 702 to a seventh heat exchanger 707, the plurality of third heat exchange devices is a ninth heat exchanger 709 to an eleventh heat exchanger 711, the fourth heat exchange device is an eighth heat exchanger 708, the plurality of first heat exchange medium storage devices is a first heat exchange medium storage tank 271 to a third heat exchange medium storage tank 273, and the second heat exchange medium storage device is a fourth heat exchange medium storage tank 274. The following is merely an example of the present invention and is not intended to limit the scope of the present invention.
As shown in fig. 2, the tank 12 for the extract is connected to the inlets of the materials of the first extraction tank 101 and the second extraction tank 102 by two branch pipes, respectively. The gaseous fluid reservoir 1 is connected to the inlet of the first filter 601 by a pipe, and a first solenoid valve 501 is provided on the pipe between the gaseous fluid reservoir 1 and the first filter 601. The outlet of the first filter 601 is connected to the inlet of the high temperature end of the first heat exchanger 701 through a pipe. The outlet of the high temperature end of the first heat exchanger 701 is connected to the inlet of the gas-liquid separation tank 2 through a pipeline. The gas phase outlet of the gas-liquid separation tank 2 at the top is connected to the inlet of the high temperature end of the first heat exchanger 701 through a pipeline, and a thirty-fourth electromagnetic valve 534 is arranged between the gas-liquid separation tank 2 and the first heat exchanger 701. The liquid phase outlet of the gas-liquid separation tank 2 at the bottom is connected to the inlet of the liquid fluid storage tank 3 through a pipeline, and a second electromagnetic valve 502 is arranged on the pipeline between the gas-liquid separation tank 2 and the liquid fluid storage tank 3. The outlet of the liquid fluid reservoir 3 is connected to the inlet of the booster pump 4 by a pipe, and a third solenoid valve 503 is provided in the pipe between the liquid fluid reservoir 3 and the booster pump 4. The outlet of the booster pump 4 is connected to the inlet of the second filter 602 through a pipe, and a fourth electromagnetic valve 504 is provided on the pipe between the booster pump 4 and the second filter 602. The outlet of the entrainer storage tank 13 is connected to the inlet of the entrainer delivery pump 15 by a pipe. The outlet of the entrainer delivery pump 15 is combined with the inlet of the second filter 602 by a pipeline, and an entrainer flowmeter 903 and a nineteenth electromagnetic valve 519 are arranged on the pipeline before the combination.
The outlet of the second filter 602 is divided into two branch pipelines connected in parallel through two pipelines, one branch pipeline is connected to the fluid inlet of the second heat exchanger 702, the other branch pipeline is connected to the fluid inlet of the fifth heat exchanger 705, a fifth electromagnetic valve 505 and a first flowmeter 901 are arranged on the pipeline between the outlet of the second filter 602 and the second heat exchanger 702, and a ninth electromagnetic valve 509 and a second flowmeter 902 are arranged on the pipeline between the second filter 602 and the fifth heat exchanger 705. The second heat exchanger 702 fluid outlet is connected to the first extraction tank 101 fluid inlet by a pipe, and the first extraction tank 101 fluid outlet is connected to the third heat exchanger 703 fluid inlet by a pipe. A sixth electromagnetic valve 506 is arranged on a pipeline between the first extraction kettle 101 and the third heat exchanger 703, a first emptying pipeline 801 is arranged below the first extraction kettle 101, and a thirteenth electromagnetic valve 513 is arranged on the first emptying pipeline 801. The third heat exchanger 703 fluid outlet is connected to the first separation tank 111 fluid inlet through a pipe, the first separation tank 111 fluid outlet is connected to the fourth heat exchanger 704 fluid inlet through a pipe, a seventh electromagnetic valve 507 is arranged on the pipe between the first separation tank 111 and the fourth heat exchanger 704, and the fourth heat exchanger 704 fluid outlet is connected to the second separation tank 112 fluid inlet through a pipe. The fifth heat exchanger 705 fluid outlet is connected to the second extraction tank 102 fluid inlet through a pipe, the second extraction tank 102 fluid outlet is connected to the sixth heat exchanger 706 fluid inlet through a pipe, a tenth electromagnetic valve 510 is arranged on the pipe between the second extraction tank 102 and the sixth heat exchanger 706, a second evacuation pipe 802 is arranged below the second extraction tank 102, and a sixteenth electromagnetic valve 516 is arranged on the second evacuation pipe 802. The sixth heat exchanger 706 fluid outlet is connected to the third separation tank 113 fluid inlet by a pipe, the third separation tank 113 fluid outlet is connected to the seventh heat exchanger 707 fluid inlet by a pipe, an eleventh solenoid valve 511 is provided on the pipe between the third separation tank 113 and the seventh heat exchanger 707, and the seventh heat exchanger 707 fluid outlet is connected to the fourth separation tank 114 fluid inlet by a pipe.
The material outlets of the first separation kettle 111 to the fourth separation kettle 114 are connected to the inlet of the gaseous fluid separation tank 16 through a pipeline in a merging way, a fourteenth electromagnetic valve 514 and a fifteenth electromagnetic valve 515 are respectively arranged at the material outlets of the first separation kettle 111 and the second separation kettle 112, and a seventeenth electromagnetic valve 517 and an eighteenth electromagnetic valve 518 are respectively arranged at the material outlets of the third separation kettle 113 and the fourth separation kettle 114; the fluid outlets of the second separation kettle 112 and the fourth separation kettle 114 are combined with the fluid outlet of the gaseous fluid separation tank 16 into one path through a pipeline, and then are combined with the pipeline at the outlet of the gaseous fluid storage tank 1, wherein an eighth electromagnetic valve 508 and a twelfth electromagnetic valve 512 are arranged at the fluid outlets of the second separation kettle 112 and the fourth separation kettle 114. The material outlet of the gaseous fluid separation tank 16 is connected by piping to a first material storage tank 171 in communication with the fractionation purification subsystem 20 a.
The outlet of the first material storage tank 171 is connected to the inlet of the first material transfer pump 261 by a pipe, the outlet of the first material transfer pump 261 is connected to the material inlet of the first distiller 181 by a pipe, and the extract outlet of the first distiller 181 is connected to the first extract storage tank 191 by a pipe. The vacuum outlet of the first distiller 181 is connected to the vacuum inlet of the first condensing chamber 201 by a pipe, the extract outlet of the first condensing chamber 201 is connected to the second extract reservoir 192 by a pipe, and the vacuum outlet of the first condensing chamber 201 is connected to the first vacuum pump 211 by a pipe. The material outlet of the first distiller 181 is connected to the inlet of the second material storage tank 172 through a pipe, the material outlet of the second material storage tank 172 is connected to the inlet of the second material transfer pump 262 through a pipe, a thirty-third electromagnetic valve 533 is arranged on the pipe between the second material storage tank 172 and the second material transfer pump 262, an evacuation branch 803 is arranged, and a thirty-second electromagnetic valve 532 is arranged on the evacuation branch 803. The outlet of the second material transfer pump 262 is connected by a pipe to the material inlet of the second distiller 182, and the extract outlet of the second distiller 182 is connected by a pipe to the third extract tank 193. The vacuum outlet of the second distiller 182 is connected by tubing to the second condensing chamber 202 vacuum inlet, the extract outlet of the second condensing chamber 202 is connected by tubing to the fourth extract tank 194, the vacuum outlet of the second condensing chamber 202 is connected by tubing to the second vacuum pump 212, and the material outlet of the second distiller 182 is connected by tubing to the material residue tank 173.
The first compressor 221 and the second compressor 222 outlet are connected to the eighth heat exchanger 708 fluid inlet by a combination of pipes, the eighth heat exchanger 708 hot water outlet is connected to the first water transfer pump 251 inlet by a pipe, the first water transfer pump 251 outlet is connected to the fourth heat exchange medium storage tank 274 hot water inlet by a pipe, and the fourth heat exchange medium storage tank 274 hot water outlet is connected to the eighth heat exchanger 708 hot water inlet by a pipe. The outlet of the circulation side of the fourth heat exchange medium storage tank 274 is connected to the inlet of the second water delivery pump 252 through a pipeline, the outlet of the second water delivery pump 252 is connected to the hot water inlet of the first distiller 181 and the hot water inlet of the second distiller 182 through pipelines respectively, a thirty-first electromagnetic valve 530 is arranged on the pipeline between the second water delivery pump 252 and the first distiller 181, a thirty-first electromagnetic valve 531 is arranged on the pipeline between the second water delivery pump 252 and the second distiller 182, and the hot water outlet of the first distiller 181 and the hot water outlet of the second distiller 182 are connected to the inlet of the circulation side of the fourth heat exchange medium storage tank 274 through pipeline combination.
The eighth heat exchanger 708 fluid outlet is connected by tubing to the ninth heat exchanger 709 fluid inlet, the ninth heat exchanger 709 hot water outlet is connected by tubing to the third water transfer pump 253 inlet, the third water transfer pump 253 outlet is connected by tubing to the first heat exchange medium reservoir 271 hot water inlet, and the first heat exchange medium reservoir 271 hot water outlet is connected by tubing to the ninth heat exchanger 709 hot water inlet. The circulation side outlet of the first heat exchange medium storage tank 271 is connected to the inlet of the fourth water transfer pump 254 through a pipe, and a twentieth electromagnetic valve 520 is provided on the pipe between the first heat exchange medium storage tank 271 and the fourth water transfer pump 254. The outlet of the fourth water transfer pump 254 is connected to the hot water inlet of the fourth heat exchanger 704 and the hot water inlet of the seventh heat exchanger 707 by two paths respectively through pipes, a twenty-first electromagnetic valve 521 is provided on the pipe between the fourth water transfer pump 254 and the fourth heat exchanger 704, and the hot water outlet of the fourth heat exchanger 704 and the hot water outlet of the seventh heat exchanger 707 are connected to the circulating side inlet of the first heat exchange medium storage tank 271 by pipe combination.
The fluid outlet of the ninth heat exchanger 709 is connected to the fluid inlet of the tenth heat exchanger 710 through a pipe, the hot water outlet of the tenth heat exchanger 710 is connected to the inlet of the fifth water transfer pump 255 through a pipe, the outlet of the fifth water transfer pump 255 is connected to the hot water inlet of the second heat exchange medium storage tank 272 through a pipe, and the hot water outlet of the second heat exchange medium storage tank 272 is connected to the hot water inlet of the tenth heat exchanger 710 through a pipe. The circulation side outlet of the second heat exchange medium storage tank 272 is connected to the inlet of the sixth water transfer pump 256 through a pipeline, a twenty-second electromagnetic valve 522 is arranged on the pipeline between the second heat exchange medium storage tank 272 and the sixth water transfer pump 256, the outlet of the sixth water transfer pump 256 is connected to the hot water inlet of the third heat exchanger 703 and the hot water inlet of the sixth heat exchanger 706 respectively through pipelines in two ways, and a twenty-third electromagnetic valve 523 is arranged on the pipeline between the sixth water transfer pump 256 and the third heat exchanger 703. The hot water outlet of the third heat exchanger 703 and the hot water outlet of the sixth heat exchanger 706 are connected to the circulation side inlet of the second heat exchange medium storage tank 272 by pipe combination.
The tenth heat exchanger 710 fluid outlet is connected to the eleventh heat exchanger 711 fluid inlet by a pipe, the eleventh heat exchanger 711 hot water outlet is connected to the seventh water transfer pump 257 inlet by a pipe, the seventh water transfer pump 257 outlet is connected to the third heat exchange medium storage tank 273 hot water inlet by a pipe, and the third heat exchange medium storage tank 273 hot water outlet is connected to the eleventh heat exchanger 711 hot water inlet by a pipe. The outlet of the circulation side of the third heat exchange medium storage tank 273 is connected to the inlet of the eighth water delivery pump 258 through a pipeline, a twenty-fourth electromagnetic valve 524 is arranged on the pipeline between the third heat exchange medium storage tank 273 and the eighth water delivery pump 258, the outlet of the eighth water delivery pump 258 is connected to the hot water inlet of the second heat exchanger 702 and the hot water inlet of the fifth heat exchanger 705 respectively through pipelines in two paths, and a twenty-fifth electromagnetic valve 525 is arranged on the pipeline between the eighth water delivery pump 258 and the second heat exchanger 702. The hot water outlet of the second heat exchanger 702 and the hot water outlet of the fifth heat exchanger 705 are connected to the circulation side inlet of the third heat exchange medium storage tank 273 by pipe merging.
The fluid outlet of the eleventh heat exchanger 711 is connected to the inlets of the first throttle expansion device 231 to the third throttle expansion device 233 respectively by three paths of pipelines; the outlet of the first throttling expansion device 231 is connected to the fluid inlet of the first carbon dioxide storage tank 141 through a pipeline; the circulation side outlet of the first carbon dioxide storage tank 141 is connected to the inlet of the first carbon dioxide delivery pump 241 through a pipe, the outlet of the first carbon dioxide delivery pump 241 is connected to the low temperature side inlet of the first heat exchanger 701 through a pipe, and the low temperature side outlet of the first heat exchanger 701 is connected to the circulation side inlet of the first carbon dioxide storage tank 141 through a pipe;
the outlet of the second throttling expansion device 232 is connected to the fluid inlet of the second carbon dioxide storage tank 142 through a pipeline, the outlet of the circulation side of the second carbon dioxide storage tank 142 is connected to the inlet of the second carbon dioxide delivery pump 242 through a pipeline, the outlet of the second carbon dioxide delivery pump 242 is respectively connected to the fluid side inlets of the first distiller 181 and the second distiller 182 through two paths through a pipeline, and a twenty-sixth electromagnetic valve 526 and a twenty-seventh electromagnetic valve 527 are respectively arranged on the pipeline between the second carbon dioxide delivery pump 242 and the first distiller 181 and the second distiller 182. The first distiller 181 fluid outlet and the second distiller 182 fluid outlet are connected by piping combination to the circulation side inlet of the second carbon dioxide storage tank 142;
The outlet of the third throttling expansion device 233 is connected to the fluid inlet of the third carbon dioxide storage tank 143 through a pipeline, the outlet of the circulation side of the third carbon dioxide storage tank 143 is connected to the inlet of the third carbon dioxide delivery pump 243 through a pipeline, the outlet of the third carbon dioxide delivery pump 243 is respectively connected to the fluid side inlets of the first condensation chamber 201 and the second condensation chamber 202 through two paths through a pipeline, and a twenty-eighth electromagnetic valve 528 and a twenty-ninth electromagnetic valve 529 are respectively arranged on the pipeline between the second carbon dioxide delivery pump 242 and the first condensation chamber 201 and the second condensation chamber 202. The first condensing chamber 201 fluid outlet and the second condensing chamber 202 fluid outlet are connected to the third carbon dioxide storage tank 143 circulation side inlet by pipe union.
The gaseous outlets of the first to third carbon dioxide tanks 141 to 143 are connected to the inlets of the first and second compressors 221 and 222 by pipe union.
According to an embodiment of the present invention, as shown in fig. 3, a control method of a processing system for extracting plant active ingredients by supercritical fluid is provided, which adopts the processing system of the above embodiment, and controls on-off of each pipeline in the processing system to achieve efficient and high-purity extraction of active ingredients, and low-energy-consumption operation of the processing system. In the embodiment, different electromagnetic valves are adopted to control the conduction of the corresponding pipelines, all the electromagnetic valves are connected to a logic circuit, the logic circuit controls the opening and closing of the electromagnetic valves, and the electromagnetic valves are matched with the logic circuit to control whether carbon dioxide or heat exchange medium can pass through the corresponding pipelines. The control method of the present embodiment includes the steps of:
S11, the first heat exchange medium circulation loop 1b, the third heat exchange medium circulation loop 3b and the first carbon dioxide circulation loop 1c of the carbon dioxide cold and heat combined supply subsystem 30a are controlled to be started.
In this embodiment, the required extraction conditions are preset before the start-up system is operated, and the extraction conditions include the outlet temperature T of the first heat exchanger 701 in combination with the processing system of fig. 2 and the control flow diagram of fig. 6 2 First extraction kettle 101 pressure P 101 And temperature T 101 Pressure P of second extraction kettle 102 102 And temperature T 102 Pressure P of first separation vessel 111 111 And temperature T 111 Pressure P of second separation tank 112 112 And temperature T 112 Pressure P of third separation tank 113 113 And temperature T 113 Pressure P of fourth separation tank 114 114 And temperature T 114 Pressure P of first distiller 181 181 And distillation temperature T h,181 Second distiller 182 pressure P 182 And temperature T h,182 Condensation temperature T of first distiller 181 and second distiller 182 c,181 And T c,182 Temperature T of the first condensation chamber 201 and the second condensation chamber 202 201 And T 202 Time t of extraction, time t of distillation in first distiller 181 181 Distillation time t of second distiller 182 182 Etc. The above extraction conditions are determined according to the type of extracted plant or the type of active ingredient to be extracted. Exemplary, T 2 The range of (C) is 8-10 ℃, P 101 20MPa, P 102 20MPa, T 102 45 ℃, P 111 6MPa, T 111 50 ℃, P 112 5.5MPa, T 112 At 55 ℃, P 113 6MPa, T 113 50 ℃, P 114 5.5MPa, T 114 At 55 ℃, P 181 500Pa, T h,181 At 55 ℃, P 182 500Pa, T h,182 At 60 ℃, T c,181 Is at 12-14 ℃, T c,182 Is at 12-14 ℃, T 201 Is 10-12 ℃, T 202 At 10-12 deg.c and t of 2-3 hrh，t 181 1h to 2h, t 182 1 to 2 hours.
After the required extraction conditions are set, the first heat exchange medium circulation loop 1b, the third heat exchange medium circulation loop 3b and the first carbon dioxide circulation loop 1c of the carbon dioxide cold and hot combined supply subsystem 30a are controlled to be started so as to preheat the heat exchange medium in the first heat exchange medium circulation loop 1b and the heat exchange medium in the third heat exchange medium circulation loop 3b and pre-cool the carbon dioxide in the first carbon dioxide circulation loop 1 c. Referring to fig. 2 and 6, the specific operations are: the first compressor 221 and the second compressor 222 are controlled to be started, and the control system automatically turns on the first water delivery pump 251, the third water delivery pump 253, the fifth water delivery pump 255 and the seventh water delivery pump 257, and turns on the first carbon dioxide delivery pump 241.
S12, controlling the supercritical fluid extraction subsystem 10a to start operating according to the condition that the temperature of the first heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem 30a reaches the first temperature condition and the temperature of the first carbon dioxide storage tank 1c reaches the second temperature condition.
In this embodiment, when the temperature of the first heat exchange medium storage device reaches the first temperature condition, it is explained that the temperature of the heat exchange medium in the first heat exchange medium circulation loop 1b reaches the condition that the carbon dioxide in the second heat exchange device can be heated to the appropriate extraction temperature or separation temperature. Meanwhile, when the temperature of the first carbon dioxide storage tank 141 reaches the second temperature condition, it is indicated that the temperature of the carbon dioxide in the first carbon dioxide circulation loop 1c reaches the temperature condition capable of condensing the gaseous carbon dioxide in the first heat exchange device into liquid carbon dioxide.
The temperature in the first heat exchange medium storage device is set as T1, the fluid outlet temperature of the second heat exchange device of the carbon dioxide cold and heat combined supply subsystem 30a corresponding to the first heat exchange medium storage device is set as T01, and the first temperature condition is as follows: t1 is more than or equal to T01+ and is at a first set temperature; the temperature of the first carbon dioxide storage tank is T2, the fluid outlet temperature of the first heat exchange device of the carbon dioxide cold and hot combined supply subsystem 30a is T02, and the second temperature condition is: t2 is more than or equal to T02-second set temperature. First and second set temperaturesThe temperatures are in the range of 0 to 8 ℃, for example, the first set temperature is 5 ℃ and the second set temperature is 5 ℃. In combination with the processing system of fig. 2 and the control flow diagram of fig. 6, T1 comprises the temperatures T of the first 271 to third 273 heat exchange medium storage tanks 271 、T 272 、T 273 T01 comprises the extraction kettle temperature T 101 First separation tank 111 temperature T 111 Temperature T of second separation tank 112 112 T2 corresponds to the temperature T of the first carbon dioxide tank 141 141 T02 corresponds to the fluid outlet temperature T of the first heat exchanger 701 2 . The first temperature conditions were: t (T) 271 ≥T 112 +5℃，T 272 ≥T 111 +5℃，T 273 ≥T 101 +5℃; the second temperature condition is T 141 ≥T 2 －5℃。
When the above temperature conditions are reached, the supercritical fluid extraction subsystem 10a is controlled to start operating to separate the first material containing the active ingredient from the material to be extracted.
S13, controlling the fractionation purification subsystem 20a to start operation so as to separate the effective components from the first material.
According to the control method of the embodiment, the processing system for extracting the plant active ingredients by the supercritical fluid is provided with reasonable control logic so as to realize the efficient, high-purity and low-energy extraction of the plant active ingredients. After the whole system is stopped, the electric control device automatically closes all the electromagnetic valves, the delivery pump and the compressor, and the electric control device is opened according to the steps S11-S13 when the electric control device starts working next time.
In accordance with an embodiment of the present invention, prior to controlling the start-up of fractionation purification subsystem 20a, the control method further comprises: controlling the entrainer subsystem 40a to activate. In combination with the processing system of fig. 2 and the control flowchart of fig. 6, before the fractionation purification subsystem 20a is turned on, the entrainer subsystem 40a is turned on according to actual requirements, if the entrainer is needed to be used, after step S12, the control system turns on the entrainer delivery pump 15 and the nineteenth electromagnetic valve 519, and when the entrainer delivery pump 15 and the nineteenth electromagnetic valve 519 are not needed to be used, the control system turns off the entrainer delivery pump 15 and the nineteenth electromagnetic valve 519.
As shown in fig. 4, in the step of controlling the supercritical fluid extraction subsystem 10a to start operation, the following steps are further included according to an embodiment of the present invention:
s21, controlling the material to be extracted to enter an extraction kettle of the supercritical fluid extraction subsystem 10a, and controlling the passage conduction between a gaseous fluid storage tank 1 and a liquid fluid storage tank 3 of the supercritical fluid extraction subsystem 10 a.
S22, controlling the second heat exchange medium circulation loop 2b of the carbon dioxide cold and hot combined supply subsystem 30a to start according to the condition that the pressure of the liquid fluid storage tank 3 reaches the first pressure, and controlling the passage conduction between the gaseous fluid storage tank 1 and the extraction kettle.
In this embodiment, the first pressure condition is the lowest pressure condition for the start-up operation of the extraction tank, and the first pressure condition is the pressure P of the liquid fluid storage tank 3 3 The set pressure is, for example, 3.5 to 5Mpa. When the pressure of the liquid fluid storage tank 3 reaches the first pressure condition, the second heat exchange medium circulation loop 2b is started, and heat exchange is carried out between the second heat exchange medium circulation loop 2b and the second heat exchange device at the inlet of the extraction kettle, so that carbon dioxide entering the second heat exchange device is heated, and the temperature of the carbon dioxide entering the extraction kettle reaches the proper extraction temperature. In combination with the processing system of fig. 2 and the control flow diagram of fig. 6, the control system automatically opens the first solenoid valve 501, the second solenoid valve 502. When the pressure P of the liquid fluid reservoir 3 3 The control system automatically opens the fourth water feed pump 254, the sixth water feed pump 256, the eighth water feed pump 258, the first solenoid valve 501 to the fifth solenoid valve 505, the twentieth solenoid valve 520 to the twenty-fifth solenoid valve 525 when the set pressure range is in.
S23, controlling carbon dioxide to flow between the gaseous fluid storage tank 1 and the extraction kettle, controlling the passage between the extraction kettle and the separation kettle of the supercritical fluid extraction subsystem 10a to be communicated according to the condition that the pressure of the extraction kettle reaches the second pressure, and maintaining the pressure of the extraction kettle at the second pressure condition.
In this embodiment, the second pressure condition is a suitable pressure condition for extracting the first material with supercritical carbon dioxide, for example, a second set pressure conditionFor the pressure of the first extraction kettle 101 to reach the set pressure P 101 The pressure of the second extraction kettle 102 reaches a set pressure P 102 . When the pressure of the extraction kettle reaches the second pressure condition, the supercritical carbon dioxide and the first material mixture enter the separation kettle by controlling the conduction of the passage between the extraction kettle and the separation kettle, and the supercritical carbon dioxide is changed into a gaseous state by the separation kettle so as to be separated from the first material. In combination with the processing system of fig. 2 and the control flow diagram of fig. 6, in particular, the control system automatically turns on the booster pump 4 when the set pressure P is reached 101 The control system automatically opens the sixth electromagnetic valve 506, and simultaneously precisely controls the pressure of the first extraction kettle 101 through the sixth electromagnetic valve 506, and maintains the pressure of the first extraction kettle 101 at P 101 Within + -0.5 MPa.
S24, controlling the passage conduction between the fluid outlet of the separation kettle and the fluid outlet of the gaseous fluid storage tank 1 according to the condition that the pressure of the separation kettle reaches the third pressure, and maintaining the pressure of the extraction kettle at the third pressure.
In this example, the third pressure condition is a pressure condition at which the separation tank starts to separate the first material from the gaseous carbon dioxide. For example, the third set pressure condition is that the pressure of the first separation tank 111 reaches the set pressure P 111 The pressure of the second separation tank 112 reaches the set pressure P 112 . When the pressure of the separation kettle reaches the third pressure condition, the gaseous carbon dioxide and the first material are separated, and the separated gaseous carbon dioxide can be discharged. In combination with the processing system of fig. 2 and the control flow diagram of fig. 6, specifically, it is determined whether the pressure of the first separation tank 111 reaches the set pressure P 111 If yes, the control system automatically opens the seventh electromagnetic valve 507, and simultaneously precisely controls the pressure of the first separation kettle 111 to be P through the seventh electromagnetic valve 507 111 Within + -0.5 MPa. Judging whether the pressure of the second separation kettle 112 reaches the set pressure P 112 If yes, the control system automatically opens the eighth electromagnetic valve 508, and simultaneously precisely controls the pressure of the second separation kettle 112 to be P through the eighth electromagnetic valve 508 112 Within + -0.5 MPa.
S25, controlling the passages between the liquid fluid storage tank 3 and the extraction kettle, between the extraction kettle and the separation kettle and between the separation kettle and the gaseous fluid storage tank 1 to be respectively disconnected according to the extraction time of the extraction kettle reaching the set extraction time, and controlling the passage between the material outlet of the separation kettle and the gaseous fluid separation tank 16 of the supercritical fluid extraction subsystem 10a to be connected.
In this embodiment, when the extraction time of the extraction kettle reaches the set extraction time, it is indicated that the first material containing the effective component in the material to be extracted is substantially extracted, and at this time, the passages between the liquid fluid storage tank 3 and the extraction kettle, between the extraction kettle and the separation kettle, and between the separation kettle and the gaseous fluid storage tank 1 need to be closed. With reference to the processing system of fig. 2 and the control flowchart of fig. 6, the electronic control device controls the extraction time of the first extraction kettle 101, and if the extraction time reaches t, the electronic control device immediately closes the fifth electromagnetic valve 505 to the eighth electromagnetic valve 508.
S26, controlling the disconnection of a passage between a material outlet of the separation kettle and the gaseous fluid separation tank 16 according to the emptying of the extract in the separation kettle, controlling the connection of an emptying pipeline of the supercritical fluid extraction subsystem 10a, and controlling the closing of the emptying pipeline according to the condition that the pressure of the extraction kettle reaches the fourth pressure.
In this embodiment, when the extract in the separation tank is exhausted, the path between the material outlet of the separation tank and the gaseous fluid separation tank 16 is disconnected, and the exhaust pipe of the extraction tank is connected to exhaust the residual carbon dioxide in the extraction tank. The fourth pressure condition is a pressure condition for evacuating carbon dioxide in the extraction kettle, for example, the fourth pressure condition is normal pressure. With reference to the processing system of fig. 2 and the control flow chart of fig. 6, the control system automatically opens the fourteenth electromagnetic valve 514 and the fifteenth electromagnetic valve 515, the extract enters the gaseous fluid separation tank 16, and the electronic control device judges whether the extracts of the first separation tank 111 and the second separation tank 112 are empty, if so, immediately closes the fourteenth electromagnetic valve 514 and the fifteenth electromagnetic valve 515. The control system automatically opens the thirteenth electromagnetic valve 513, and the electric control device judges whether the pressure of the first extraction kettle 101 reaches the fourth pressure condition, if so, the thirteenth electromagnetic valve 513 is closed.
In this embodiment, when the supercritical fluid extraction subsystem 10a includes two extraction separation units connected in parallel, the material is filled into the second extraction kettle 102 from the storage tank 12 to be extracted through the control system, and the control steps after the material enters the second extraction kettle 102 are the same as those of steps S23 to S26, which are not described herein again. It should be noted that, the control steps of the two extraction separation units may be performed simultaneously or sequentially, and may be selected according to actual needs.
As shown in fig. 5, controlling the start-up of the fractionation purification subsystem 20a according to an embodiment of the present invention includes the steps of:
s31, controlling the fourth heat exchange medium circulation loop 4b of the carbon dioxide cold and hot combined supply subsystem 30a to start according to the condition that the temperature of the second heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem 30a reaches the third temperature.
In this embodiment, the third temperature condition is a temperature at which the temperature of the heat exchange medium in the fourth heat exchange medium circulation loop 4b can vaporize the active ingredient in the first material. The temperature of the second heat exchange medium storage device is T3, the distillation temperature of the distiller is T03, and the third temperature condition is: t3 is more than or equal to T03+ and the third set temperature. The third set temperature is, for example, 0 to 8 ℃, e.g., the third set temperature is 5 ℃. When the temperature of the second heat exchange medium storage device reaches the third temperature condition, the fourth heat exchange medium circulation loop 4b is controlled to start so as to vaporize the effective components in the first material entering the distiller. Combining the processing system of fig. 2 and the control flow diagram of fig. 6, T3 corresponds to the fourth heat exchange medium tank T 274 T03 corresponds to the distillation temperature T of the first distiller 181 h,181 Judgment of T 274 ≥T h,181 If the +5℃ condition is met, the control system automatically opens the second water transfer pump 252, the thirty-first solenoid valve 530, and the thirty-first solenoid valve 531.
S32, controlling the second carbon dioxide circulation loop 2c and the third carbon dioxide circulation loop 3c of the carbon dioxide cold and hot combined supply subsystem 30a to start according to the condition that the temperature of the second carbon dioxide storage tank 142 of the carbon dioxide cold and hot combined supply subsystem 30a reaches the fourth temperature condition and the temperature of the third carbon dioxide storage tank 143 reaches the fifth temperature condition.
This embodimentThe fourth temperature condition is a proper temperature at which the carbon dioxide in the second carbon dioxide circulation circuit 2c can condense the vaporized active ingredient in the first condensation unit 1a, and the fifth temperature condition is a proper temperature at which the carbon dioxide in the third carbon dioxide circulation circuit 3c can condense the vaporized active ingredient in the second condensation unit 2 a. The temperature of carbon dioxide in the second carbon dioxide storage tank 142 is T4, the condensing temperature of the distiller is T04, and the fourth temperature condition is: t4 is more than or equal to T04+ and is at a fourth set temperature. The temperature of the third carbon dioxide tank 143 is T5, the temperature of the condensing chamber is T05, and the fifth temperature condition is: t5 is greater than or equal to T05 and is at a fifth set temperature. Illustratively, the fourth set temperature and the fourth set temperature are both 0-8 ℃, e.g., the fourth set temperature is 5 ℃, and the fifth set temperature is 5 ℃. After the temperature of the second carbon dioxide tank 142 reaches the fourth temperature condition and the temperature of the third carbon dioxide tank 143 reaches the fifth temperature condition, the second carbon dioxide circulation loop 2c and the third carbon dioxide circulation loop 3c are controlled to be started so as to condense the vaporized active ingredients in the first condensation part 1a and the second condensation part 2 a. Combining the processing system of fig. 2 and the control flow diagram of fig. 6, T4 corresponds to the temperature T of the second carbon dioxide storage tank 142 142 T5 corresponds to the temperature T of the third carbon dioxide tank 143 143 T04 corresponds to the condensation temperature T of the first distiller 181 c,181 T05 corresponds to the condensation temperature T of the first condensation chamber 201 201 . Judgment T 142 ≥T c,181 +5℃、T 143 ≥T 201 If the +5 ℃ condition is met, the control system automatically opens the second 242 and third 243 carbon dioxide transfer pumps, twenty-sixth 526 to twenty-ninth 529 solenoid valves.
And S33, controlling the vacuum pump of the fractionation purification subsystem 20a to be started, and controlling the first material storage tank 171 of the supercritical fluid extraction subsystem 10a to convey the first material to the distiller according to the condition that the pressure of the distiller of the fractionation purification subsystem 20a reaches the fifth pressure.
In this embodiment, the fifth pressure condition is a pressure condition in which the pressure in the distiller reaches a pressure condition that allows vaporization of the active ingredient in the first material. The first pressure condition is that the pressure of the distiller reaches the set valueConstant pressure. In combination with the processing system of fig. 2 and the control flowchart of fig. 6, the control system automatically turns on the first vacuum pump 211 and the second vacuum pump 212, and the electronic control device determines whether the pressures of the first distiller 181 and the second distiller 182 reach the set pressure P 181 And P 182 If so, the control system automatically turns on the first material transfer pump 261.
And S34, controlling the communication between the distiller and the second material storage tank 172 of the fractional purification subsystem 20a according to the distillation time of the distiller reaching the set distillation time.
In this embodiment, when the distillation time of the distiller reaches the set distillation time, it is indicated that the effective components of the first material in the distiller are mostly vaporized, and the unvaporized second material needs to be discharged into the second material storage tank 172 for reuse or entering the next round of distillation process. With reference to the processing system of fig. 2 and the control flowchart of fig. 6, the electronic control unit determines whether the distillation time of the first distiller 181 reaches t 181 If so, the control system automatically opens the thirty-third solenoid valve 533 and the second material transfer pump 262, and then performs continuous operation.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (13)
1. A processing system for extracting plant active ingredients by supercritical fluid, which is characterized by comprising a supercritical fluid extraction subsystem, a fractionation purification subsystem and a carbon dioxide cold and hot combined supply subsystem; wherein,,
The supercritical fluid extraction subsystem is used for separating a first material containing active ingredients from a material to be extracted by utilizing supercritical carbon dioxide; the supercritical fluid extraction subsystem comprises a first fluid branch and a second fluid branch which are connected in series along the flow direction of the carbon dioxide;
the fractionation purification subsystem is connected in series with the second fluid branch and is used for purifying the effective components in the first material; the fractionation purification subsystem comprises a vaporization part and a condensation part;
the carbon dioxide cold and hot combined supply subsystem comprises a compression unit, a first heat supply unit, a second heat supply unit, a first cooling unit and a second cooling unit; the compression unit, the first heat supply unit and the second heat supply unit are sequentially connected in series along the flowing direction of carbon dioxide; the first cooling unit and the second cooling unit are connected in parallel, an inlet of a parallel passage of the first cooling unit and the second cooling unit is communicated with the second heat supply unit, and an outlet of a parallel passage of the first cooling unit and the second cooling unit is communicated with the compression unit;
the first cooling unit exchanges heat with the first fluid branch so as to condense gaseous carbon dioxide in the first fluid branch into liquid carbon dioxide; the second heat supply unit exchanges heat with the second fluid branch so as to heat supercritical carbon dioxide in the second fluid branch to reach a preset extraction temperature or separation temperature; the first heat supply unit is in heat exchange with the vaporizing part so as to vaporize the effective components in the first material entering the vaporizing part; and the second cooling unit is in heat exchange with the condensing part so as to condense the vaporized active ingredients.
2. The processing system for extracting plant active ingredients with supercritical fluid according to claim 1, wherein the supercritical fluid extraction subsystem comprises a to-be-extracted storage tank, a gaseous fluid storage tank, a first heat exchange device, a gas-liquid separation tank, a liquid fluid storage tank, an extraction separation unit, a gaseous fluid separation tank and a first material storage tank; the gaseous fluid storage tank, the first heat exchange device, the gas-liquid separation tank and the liquid fluid storage tank are sequentially connected in series on the first fluid branch along the flowing direction of carbon dioxide; the gaseous fluid outlet of the gas-liquid separation tank is communicated with the fluid inlet of the first heat exchange device; the extraction separation unit is arranged on the second fluid branch, and the storage tank for the to-be-extracted matters is communicated with the material inlet of the extraction separation unit; the material outlet of the extraction separation unit is communicated with the gaseous fluid separation tank, and the material outlet of the gaseous fluid separation tank is communicated with the first material storage tank; the fluid outlet of the extraction separation unit and the fluid outlet of the gaseous fluid separation tank are communicated with the outlet of the gaseous fluid storage tank;
the first cooling unit comprises a first throttling expansion device and a first carbon dioxide storage tank which are connected in series, a fluid inlet of the first throttling expansion device is communicated with the second heating unit, and a fluid outlet of the first carbon dioxide storage tank is communicated with the compression unit; and a first carbon dioxide circulation loop is formed between the first carbon dioxide storage tank and the first heat exchange device.
3. The processing system for extracting plant active ingredients from a supercritical fluid according to claim 2, wherein the extraction separation unit comprises an extraction kettle, at least one separation kettle and a plurality of second heat exchange devices, wherein the extraction kettle is connected in series with the at least one separation kettle along the flow direction of carbon dioxide, and the plurality of second heat exchange devices are respectively arranged at fluid inlets of the extraction kettle and the at least one separation kettle; the material outlet of the storage tank for the to-be-extracted substances is communicated with the material inlet of the extraction kettle; the material outlet of the separation kettle is communicated with the gaseous fluid separation tank, and the fluid outlet of the separation kettle is communicated with the outlet of the gaseous fluid storage tank; an evacuation pipeline is arranged at the bottom of the extraction kettle;
the second heat supply unit comprises a plurality of third heat exchange devices and a plurality of first heat exchange medium storage devices, and the third heat exchange devices are connected in series; the third heat exchange device is arranged corresponding to the first heat exchange medium storage device, and the first heat exchange medium storage device is arranged corresponding to the second heat exchange device; a first heat exchange medium circulation loop is formed between the third heat exchange device and the corresponding first heat exchange medium storage device, and a second heat exchange medium circulation loop is formed between the first heat exchange medium storage device and the corresponding second heat exchange device.
4. A processing system for extracting plant active ingredients by supercritical fluid according to claim 3, wherein the processing system comprises a plurality of extraction separation units, the extraction separation units are connected in parallel, the material outlet of the storage tank for the to-be-extracted substance is respectively communicated with the material inlets of the extraction separation units, the material outlets of the extraction separation units are respectively communicated with the gaseous fluid separation tank, and the fluid outlets of the extraction separation units are respectively communicated with the outlet of the gaseous fluid storage tank;
and the second heat exchange medium circulation loops are respectively formed between the first heat exchange medium storage device and the second heat exchange devices corresponding to the extraction separation units.
5. A processing system for extracting plant active ingredients from a supercritical fluid according to claim 3, wherein the fractionation purification subsystem comprises at least one distiller and at least one condensing chamber, the distiller being disposed in correspondence with the condensing chamber; the material outlet of the first material storage tank is communicated with the material inlet of the distiller, the vaporization part is positioned on the distiller, and the material inlet of the distiller is arranged on the vaporization part; the vacuum outlet of the distiller is communicated with the vacuum inlet corresponding to the condensing chamber, and the vacuum outlet of the condensing chamber is connected with a vacuum pump; the extract outlet of the distiller and the extract outlet of the condensing chamber are respectively connected with an extract storage tank, and the material outlet of the distiller is connected with a second material storage tank; the condensing part comprises a first condensing part and a second condensing part, the first condensing part is positioned on the distiller, and an extract outlet of the distiller is arranged on the first condensing part; the second condensing part is positioned on the condensing chamber, and an extract outlet of the condensing chamber is arranged on the second condensing part;
The first heat supply unit comprises a fourth heat exchange device and a second heat exchange medium storage device, a third heat exchange medium circulation loop is formed between the fourth heat exchange device and the second heat exchange medium storage device, and a fourth heat exchange medium circulation loop is formed between the second heat exchange medium storage device and the vaporization part;
the second cooling unit comprises a first cooling subunit and a second cooling subunit which are connected in parallel; the inlets of the first cooling subunit and the second cooling subunit parallel passages are communicated with the second heat supply unit, and the outlets of the first cooling subunit and the second cooling subunit parallel passages are communicated with the compression unit; the first cooling subunit comprises a second throttling expansion device and a second carbon dioxide storage tank which are connected in series along the flowing direction of carbon dioxide, and a second carbon dioxide circulation loop is formed between the second carbon dioxide storage tank and the first condensing part; the second cooling subunit comprises a third throttling expansion device and a third carbon dioxide storage tank which are connected in series, and a third carbon dioxide circulation loop is formed between the third carbon dioxide storage tank and the second condensation part.
6. The processing system for extracting plant active ingredients from a supercritical fluid of claim 5, wherein said fractionation purification subsystem comprises a plurality of said distillers and a plurality of said condensing chambers;
The plurality of distillers are connected in series step by step, the material outlet of the first material storage tank is communicated with the material inlet of the distiller positioned at the first stage, the material outlet of each distiller is respectively connected with the second material storage tank, the material outlet of the second material storage tank positioned at the upper stage is communicated with the material inlet of the distiller positioned at the lower stage, and an emptying branch is further arranged on a connecting pipeline between the material outlet of the second material storage tank and the material inlet of the distiller positioned at the lower stage;
the second heat exchange medium storage device and the vaporization parts of the plurality of distillers respectively form the fourth heat exchange medium circulation loop; the second carbon dioxide circulation loops are respectively formed between the second carbon dioxide storage tank and the first condensation parts of the plurality of distillers; and the third carbon dioxide circulating loops are respectively formed between the third carbon dioxide storage tank and the second condensing parts of the condensing chambers.
7. The processing system for extracting plant active ingredients from a supercritical fluid of claim 5, wherein the processing system comprises a first filter and a second filter; the first filter is arranged on a pipeline between the gaseous fluid storage tank and the first heat exchange device, and a fluid outlet of the extraction separation unit and a fluid outlet of the gaseous fluid separation tank are communicated with the pipeline between the first filter and the gaseous fluid storage tank; the gaseous fluid outlet of the gas-liquid separation tank is connected to a pipeline between the first heat exchange device and the first filter; the second filter is arranged on a pipeline between the liquid fluid storage tank and the extraction separation unit; a booster pump is further arranged on a pipeline between the liquid fluid storage tank and the second filter;
The processing system further includes an entrainer subsystem including an entrainer reservoir and an entrainer delivery pump; the outlet of the entrainer storage tank is connected to a pipeline between the booster pump and the second filter through an entrainer delivery pipeline, and the entrainer delivery pump is arranged on the entrainer delivery pipeline.
8. A control method of a processing system for extracting plant active ingredients with a supercritical fluid, characterized in that it is implemented by the processing system for extracting plant active ingredients with a supercritical fluid according to any one of claims 1 to 7; the control method comprises the following steps:
the method comprises the steps of controlling a first heat exchange medium circulation loop, a third heat exchange medium circulation loop and a first carbon dioxide circulation loop of the carbon dioxide cold and hot combined supply subsystem to start;
controlling the supercritical fluid extraction subsystem to start to operate according to the condition that the temperature of a first heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem reaches a first temperature condition and the temperature of a first carbon dioxide storage tank reaches a second temperature condition;
and controlling the fractionation and purification subsystem to start operation.
9. The method of claim 8, wherein the step of controlling the operation of the supercritical fluid extraction subsystem comprises:
Controlling a material to be extracted to enter an extraction kettle of the supercritical fluid extraction subsystem, and controlling a passage between a gaseous fluid storage tank and a liquid fluid storage tank of the supercritical fluid extraction subsystem to be communicated;
according to the condition that the pressure of the liquid fluid storage tank reaches a first pressure, controlling a second heat exchange medium circulation loop of the carbon dioxide cold and hot combined supply subsystem to start, and controlling a passage between the gaseous fluid storage tank and the extraction kettle to be communicated;
controlling the flow of carbon dioxide between the gaseous fluid storage tank and the extraction kettle, controlling the passage conduction between the extraction kettle and the separation kettle of the supercritical fluid extraction subsystem according to the condition that the pressure of the extraction kettle reaches a second pressure, and maintaining the pressure of the extraction kettle at the second pressure;
controlling the passage conduction between the fluid outlet of the separation kettle and the fluid outlet of the gaseous fluid storage tank according to the condition that the pressure of the separation kettle reaches the third pressure, and maintaining the pressure of the extraction kettle under the third pressure condition;
according to the extraction time of the extraction kettle reaching the set extraction time, controlling the passages between the liquid fluid storage tank and the extraction kettle, between the extraction kettle and the separation kettle and between the separation kettle and the gaseous fluid storage tank to be respectively disconnected, and controlling the material outlet of the separation kettle to be communicated with the passage between the gaseous fluid separation tank of the supercritical fluid extraction subsystem;
And controlling the disconnection of a passage between a material outlet of the separation kettle and the gaseous fluid separation tank according to the emptying of the extract in the separation kettle, controlling the connection of an emptying pipeline of the supercritical fluid extraction subsystem, and controlling the closing of the emptying pipeline according to the condition that the pressure of the extraction kettle reaches the fourth pressure.
10. The method according to claim 8, wherein the temperature of the first heat exchange medium storage device is T1, the fluid outlet temperature of the second heat exchange device of the carbon dioxide combined heat and cold supply subsystem corresponding to the first heat exchange medium storage device is T01, and the first temperature condition is: t1 is more than or equal to T01+ and is at a first set temperature;
the temperature of the first carbon dioxide storage tank is T2, the fluid outlet temperature of the first heat exchange device of the carbon dioxide cold and hot combined supply subsystem is T02, and the second temperature condition is as follows: t2 is more than or equal to T02-second set temperature.
11. The method of claim 8, wherein the step of controlling the start-up of the fractionation purification subsystem comprises:
Controlling a fourth heat exchange medium circulation loop of the carbon dioxide cold and hot combined supply subsystem to start according to the condition that the temperature of a second heat exchange medium storage device of the carbon dioxide cold and hot combined supply subsystem reaches a third temperature;
controlling a second carbon dioxide circulation loop and a third carbon dioxide circulation loop of the carbon dioxide cold and hot combined supply subsystem to start according to the condition that the temperature of a second carbon dioxide storage tank of the carbon dioxide cold and hot combined supply subsystem reaches a fourth temperature condition and the temperature of a third carbon dioxide storage tank reaches a fifth temperature condition;
controlling a vacuum pump of the fractionation and purification subsystem to start, and controlling a first material storage tank of the supercritical fluid extraction subsystem to convey a first material to a distiller of the fractionation and purification subsystem according to a fifth pressure condition reached by the pressure of the distiller;
and controlling the communication between the distiller and a second material storage tank of the fractional distillation and purification subsystem according to the distillation time of the distiller reaching the set distillation time.
12. The method according to claim 11, wherein the temperature of the second heat exchange medium storage device is T3, the distillation temperature of the distiller is T03, and the third temperature condition is: t3 is more than or equal to T03+ and is at a third set temperature;
The temperature of the second carbon dioxide storage tank is T4, the condensation temperature of the distiller is T04, and the fourth temperature condition is: t4 is more than or equal to T04+ and is at a fourth set temperature;
the temperature of the third carbon dioxide storage tank is T5, the temperature of the condensing chamber is T05, and the fifth temperature condition is: t5 is greater than or equal to T05 and is at a fifth set temperature.
13. The method of controlling a processing system for extracting plant active ingredients from a supercritical fluid according to claim 8, wherein prior to the step of controlling the start-up of the fractionation purification subsystem, the method of controlling further comprises: controlling the entrainer subsystem start-up of the processing system.
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| CN117225004A (en) * | 2023-11-14 | 2023-12-15 | 湖南禧又多油脂有限公司 | Automatic control system for vegetable oil low-temperature extraction treatment based on Internet of things |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117225004A (en) * | 2023-11-14 | 2023-12-15 | 湖南禧又多油脂有限公司 | Automatic control system for vegetable oil low-temperature extraction treatment based on Internet of things |
| CN117225004B (en) * | 2023-11-14 | 2024-01-26 | 湖南禧又多油脂有限公司 | Automatic control system for vegetable oil low-temperature extraction treatment based on Internet of things |
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