CN112473169A - Supercritical carbon dioxide extraction reaction system - Google Patents

Supercritical carbon dioxide extraction reaction system Download PDF

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Publication number
CN112473169A
CN112473169A CN202011416796.0A CN202011416796A CN112473169A CN 112473169 A CN112473169 A CN 112473169A CN 202011416796 A CN202011416796 A CN 202011416796A CN 112473169 A CN112473169 A CN 112473169A
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China
Prior art keywords
extraction
carbon dioxide
kettle
cauldron
supercritical carbon
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CN202011416796.0A
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Chinese (zh)
Inventor
陈昱
杜荣欣
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Nantong Haijia Itelligent Technology Co ltd
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Nantong Haijia Itelligent Technology Co ltd
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Priority to CN202011416796.0A priority Critical patent/CN112473169A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes

Abstract

The invention provides a supercritical carbon dioxide extraction reaction system, which comprises a gaseous carbon dioxide storage tank, a condensation system, an extraction system and a recovery system which are sequentially connected, wherein a gas-liquid separator is arranged in front of a condenser in the condensation system to separate water vapor from carbon dioxide gas, so that the ice blockage phenomenon of the condenser is avoided; the single-unit single control and the multi-unit combined control can be realized through the set linkage type extraction kettle group in the extraction system without a centralized control system, and when one reaction kettle is in a state, the work of other reaction kettles cannot be influenced, so that the work is more flexible and the reliability is better; recovery system makes the pressure in the extraction cauldron reach balanced state through the low pressure balancing unit and the separating mechanism that set up, and the extraction effect is better, has also improved the rate of recovery of carbon dioxide.

Description

Supercritical carbon dioxide extraction reaction system
Technical Field
The invention relates to the field of supercritical extraction, in particular to a supercritical carbon dioxide extraction reaction system.
Background
The supercritical carbon dioxide fluid extraction process is a new extraction process, compared with the solvent extraction method which is most widely applied at present, the solvent carbon dioxide used in the process is an inert gas, is colorless, nontoxic, tasteless, safe, environment-friendly and pollution-free, the whole extraction process is carried out at a lower temperature, and the supercritical carbon dioxide fluid extraction process has a very good protection effect on heat-sensitive, easily oxidized and volatilized substances, and is simpler and more convenient to operate, so that the supercritical carbon dioxide fluid extraction process is widely advocated.
However, in the existing supercritical carbon dioxide extraction reaction equipment, the phenomenon of ice blockage often occurs when carbon dioxide is introduced into a condenser, the work of the reaction kettles is mostly regulated and controlled by a series connection and a centralized control system, the reliability of the centralized control system is poor, the overall situation is influenced once the extraction kettles fail, great loss is caused, in addition, the unbalanced pressure extraction effect is not ideal during the extraction reaction, and the recovery rate of the carbon dioxide is low after the extraction reaction is finished.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in the existing supercritical carbon dioxide extraction reaction equipment, the phenomenon of ice blockage frequently occurs when carbon dioxide is introduced into a condenser, the work of reaction kettles is mostly regulated and controlled by a series connection and a centralized control system, the reliability of the centralized control system is poor, the overall situation is influenced once the system fails, and great loss is caused.
The technical scheme adopted by the invention for solving the technical problems is as follows: a supercritical carbon dioxide extraction reaction system comprises a gaseous carbon dioxide storage tank, a condensing system, an extraction system and a recovery system which are sequentially connected, wherein the condensing system comprises a filter, a first gas-liquid separator, a condenser and a first liquid carbon dioxide storage tank, and the filter, the first gas-liquid separator, the condenser and the first liquid carbon dioxide storage tank are sequentially connected; the extraction system comprises a main pump, a purifier and a linkage type extraction kettle group, wherein the main pump purifier and the linkage type extraction kettle group are sequentially connected, and supercritical carbon dioxide in the first liquid carbon dioxide storage tank is extracted by driving the main pump and is transmitted to the linkage type extraction kettle group to perform supercritical extraction reaction; the recovery system comprises a separation mechanism and a low-pressure balancing device, the separation mechanism is connected with the linkage type extraction kettle set and used for separating impurities from recovered carbon dioxide, and the low-pressure balancing device is connected with the linkage type extraction kettle set and used for balancing pressure in the extraction kettle during extraction.
Further: the first gas-liquid separator comprises a tank body, a plurality of metal balls arranged in the tank body and heat exchange tubes arranged on the periphery of the tank body, and a drain valve is arranged at the bottom of the tank body.
Further: the heat exchange tube is provided with an upper connector and a lower connector, and the upper connector and the lower connector are communicated with the shell pass of the condenser.
Further: linkage type extraction cauldron group includes first extraction cauldron, second extraction cauldron and third extraction cauldron, first extraction cauldron, second extraction cauldron and third extraction cauldron the input with all be equipped with the connecting pipe between the output of clarifier, and, first extraction cauldron the output with be equipped with the connecting pipe between the input of second extraction cauldron, the second extraction cauldron the output with be equipped with the connecting pipe between the input of third extraction cauldron, the third extraction cauldron the output with be equipped with the connecting pipe between the input of first extraction cauldron.
Further: the output end of the condenser is connected with a second liquid carbon dioxide storage tank, and the second liquid carbon dioxide storage tank is connected with the linkage type extraction kettle set through an auxiliary pump.
Further: the separation mechanism comprises a first heat exchanger, a second heat exchanger, a first-stage separation kettle and a second-stage separation kettle, wherein the first heat exchanger, the first-stage separation kettle, the second heat exchanger and the second-stage separation kettle are sequentially connected in series.
Further: the output ends of the first extraction kettle, the second extraction kettle and the third extraction kettle are all provided with an A interface.
Further: the recovery system is further provided with a second gas-liquid separator and a recovery tank, the input end of the second gas-liquid separator is connected with the interface A, the output end of the second gas-liquid separator is connected with the input end of the low-pressure balancing device, and the recovery tank is connected with the low-pressure balancing device and the output end of the separation mechanism.
Further: and a metal rotor flowmeter is arranged between the separation mechanism and the recovery tank.
The supercritical carbon dioxide extraction reaction system has the beneficial effects that the gas-liquid separator is arranged in front of the condenser to separate water vapor from carbon dioxide gas, so that the ice blockage phenomenon of the condenser is avoided; the single-unit single control and the multi-unit combined control can be realized through the set linkage type extraction kettle group without a centralized control system, and when one reaction kettle is in a state, the work of other reaction kettles cannot be influenced, so that the work is more flexible and the reliability is better; through the low pressure balancing unit and the separating mechanism that set up, make the pressure in the extraction cauldron reach balanced state, extract the effect better, also improved the rate of recovery of carbon dioxide.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic diagram of a supercritical carbon dioxide extraction reaction system according to the present invention;
fig. 2 is a schematic view of the structure of the first gas-liquid separator.
In the figure, 1, a gaseous carbon dioxide storage tank, 2, a filter, 3, a first gas-liquid separator, 4, a condenser, 5, a first liquid carbon dioxide storage tank, 6, a main pump, 7, a purifier, 8, a low-pressure balancing device, 9, a tank body, 10, a metal ball, 11, a heat exchange pipe, 12, a drain valve, 13, a first extraction kettle, 14, a second extraction kettle, 15, a third extraction kettle, 16, a second liquid carbon dioxide storage tank, 17, an auxiliary pump, 18, a first heat exchanger, 19, a second heat exchanger, 20, a first-stage separation kettle, 21, a second-stage separation kettle, 22, a second gas-liquid separator, 23, a recovery tank, 24 and a metal rotor flow meter are arranged.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention. On the contrary, the embodiments of the invention include all changes, modifications and equivalents coming within the spirit and terms of the claims appended hereto.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on the orientations and positional relationships shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be considered as limiting the present invention.
Furthermore, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Any process or method descriptions in flow charts or otherwise described herein may be understood as representing modules, segments, or portions of code which include one or more executable instructions for implementing specific logical functions or steps of the process, and alternate implementations are included within the scope of the preferred embodiment of the present invention in which functions may be executed out of order from that shown or discussed, including substantially concurrently or in reverse order, depending on the functionality involved, as would be understood by those reasonably skilled in the art of the present invention.
As shown in fig. 1, the invention provides a supercritical carbon dioxide extraction reaction system, which comprises a gaseous carbon dioxide storage tank condensing system, an extraction system and a recovery system, which are connected in sequence, wherein the condensing system comprises a filter 2, a first gas-liquid separator 3, a condenser 4 and a first liquid carbon dioxide storage tank 5, and the filter 2, the first gas-liquid separator 3, the condenser 4 and the first liquid carbon dioxide storage tank 5 are connected in sequence; the extraction system comprises a main pump 6, a purifier 7 and a linkage type extraction kettle group, wherein the purifier 7 of the main pump 6 and the linkage type extraction kettle group are sequentially connected, and supercritical carbon dioxide in the first liquid carbon dioxide storage tank 5 is extracted by driving the main pump 6 and is transmitted to the linkage type extraction kettle group to perform supercritical extraction reaction; the recovery system comprises a separation mechanism and a low-pressure balancing device 8, the separation mechanism is connected with the linkage type extraction kettle set and used for separating impurities from recovered carbon dioxide, and the low-pressure balancing device 8 is connected with the linkage type extraction kettle set and used for balancing pressure in the extraction kettle during extraction.
During operation, heat gaseous carbon dioxide storage tank 1 earlier, gaseous carbon dioxide's output can accelerate, get into filter 2 through the pipeline and get rid of some impurity, reentry first gas-liquid separator 3 in, can carry out and the condensation through first gas-liquid separator 3, with the vapor liquefaction and the separation of thoughtlessly having in the gaseous carbon dioxide, then in getting into condenser 4 with gaseous carbon dioxide liquefaction deposit into first liquid carbon dioxide storage tank 5, compare with current condensing system, the first gas-liquid separator 3 of setting separates the vapor liquefaction and can prevent that condenser 4 from taking place the ice jam phenomenon.
A main pump 6 in the extraction system is used as a power source to extract supercritical carbon dioxide in a first liquid carbon dioxide storage tank 5, the purity of the liquid carbon dioxide is improved through a purifier 7, and then the liquid carbon dioxide enters a reaction kettle. When the extraction reaction is carried out, the extraction kettle is communicated with the low-pressure balancing device 8, the carbon dioxide after extraction is collected, the pressure balance when the extraction effect in the extraction kettle is the best is achieved, the extraction kettle is communicated with the separation mechanism after the extraction is finished, and the residual carbon dioxide in the extraction kettle is collected and the impurities mixed in the carbon dioxide are separated.
The first gas-liquid separator 3 comprises a tank body 9, a plurality of metal balls 10 arranged in the tank body 9 and heat exchange tubes 11 arranged on the periphery of the tank body 9, and a drain valve 12 is arranged at the bottom of the tank body 9. The condensed fluid is introduced into the heat exchange tube 11, the internal temperature of the gas-liquid separator is reduced, the gaseous carbon dioxide enters the gas-liquid separator to liquefy the water vapor, when contacting the iron balls connected in series, the liquefied water vapor is adsorbed on the surfaces of the iron balls, the reason that the surface area of the balls is larger than that of the balls in other shapes, the contacted surfaces are also large, more liquefied water vapor can be adsorbed, and therefore the water vapor is separated from the carbon dioxide gas,
the heat exchange tube 11 is provided with an upper connector and a lower connector, the upper connector and the lower connector are both communicated with the shell pass of the condenser 4, so that the heat exchange tube 11 is communicated with the shell pass of the condenser 4, namely, the cooling liquid in the heat exchange tube 11 can flow into a storage chamber of the cooling liquid in the condenser 4, the cooling liquid in the condenser 4 can also enter the heat exchange tube 11, when the cooling liquid is replaced, the cooling liquid outlet at the bottom end of the condenser 4 is only required to be opened, and the cooling liquid in the gas-liquid separator can flow out when flowing into the condenser 4, so that the replacement of the cooling liquid in the gas-liquid separator is facilitated.
Linkage type extraction cauldron group includes first extraction cauldron 13, second extraction cauldron 14 and third extraction cauldron 15, first extraction cauldron 13, second extraction cauldron 14 and third extraction cauldron 15's input with all be equipped with the connecting pipe between the output of clarifier 7, and, first extraction cauldron 13's output with be equipped with the connecting pipe between the input of second extraction cauldron 14, second extraction cauldron 14's output with be equipped with the connecting pipe between the input of third extraction cauldron 15, third extraction cauldron 15's output with be equipped with the connecting pipe between the input of first extraction cauldron 13.
Set up the intercommunication of stop valve control connecting pipe or close on the connecting pipe, and then control first reation kettle, work between second reation kettle and the third reation kettle, a single many combinations of single-unit accuse have been formed, need not centralized control system alright realize the supercritical static reaction of many coordinated type, this kind of many coordinated type is compared in the connected mode of current a plurality of reation kettle series connection, reduce carbon dioxide's dwell time, every reation kettle's work efficiency has all obtained the promotion, and as a reation kettle situation, also can not influence other reation kettle's work, make work more nimble, the reliability is better.
The output end of the condenser 4 is connected with a second liquid carbon dioxide storage tank 16, the second liquid carbon dioxide storage tank 16 is connected with the linkage type extraction kettle set through an auxiliary pump 17, the second liquid carbon dioxide storage tank and the auxiliary pump 17 are connected with the reaction kettle set to form an auxiliary line, and the auxiliary line is used for driving the auxiliary pump 17 to extract the supercritical carbon dioxide in the second liquid carbon dioxide storage tank for supplying when the supercritical carbon dioxide in the first liquid carbon dioxide storage tank 5 is insufficient or a large amount of supercritical carbon dioxide needs to be filled.
The separation mechanism comprises a first heat exchanger 18, a second heat exchanger 19, a first-stage separation kettle 20 and a second-stage separation kettle 21, wherein the first heat exchanger 18, the first-stage separation kettle 20, the second heat exchanger 19 and the second-stage separation kettle 21 are sequentially connected in series. The carbon dioxide gas discharged from the reaction kettle can be mixed with some impurities, the temperature of the carbon dioxide is regulated by the first heat exchanger 18, the carbon dioxide enters the first-stage separation kettle 20 to separate a part of impurities, the temperature of the carbon dioxide is further regulated by the second heat exchanger 19, the carbon dioxide enters the second-stage separation kettle 21 to separate the rest impurities, and finally the impurities enter the recovery tank 23, so that the purity of the recovered carbon dioxide can be improved, and the carbon dioxide can be recycled conveniently.
First extraction cauldron 13, second extraction cauldron 14 and third extraction cauldron 15's output all is provided with the A interface, recovery system still is provided with second vapour and liquid separator 22 and retrieves jar 23, second vapour and liquid separator 22's input with A interface connection, its output with low pressure balancing unit 8's input is connected, retrieve jar 23 all with low pressure balancing unit 8 with separating mechanism's output is connected. Supercritical carbon dioxide can be mixed with vapor after extraction reaction in reation kettle, when passing through second vapour and liquid separator 22, can separate out vapor liquefaction from carbon dioxide gas, avoids producing ponding in the low pressure balancing unit 8, influences the life of device, also improves the purity of carbon dioxide in recovery tank 23.
And a metal rotor flowmeter 24 is arranged between the separation mechanism and the recovery tank 23 and used for monitoring the flow velocity of the carbon dioxide in the recovery pipeline and calculating the recovery rate of the carbon dioxide.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, a schematic representation of the term does not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.

Claims (9)

1. A supercritical carbon dioxide extraction reaction system is characterized in that: comprises a gaseous carbon dioxide storage tank (1), a condensing system, an extraction system and a recovery system which are connected in sequence,
the condensation system comprises a filter (2), a first gas-liquid separator (3), a condenser (4) and a first liquid carbon dioxide storage tank (5), wherein the filter (2), the first gas-liquid separator (3), the condenser (4) and the first liquid carbon dioxide storage tank (5) are sequentially connected;
the extraction system comprises a main pump (6), a purifier (7) and a linkage type extraction kettle group, wherein the purifier (7) of the main pump (6) and the linkage type extraction kettle group are sequentially connected, and supercritical carbon dioxide in the first liquid carbon dioxide storage tank (5) is extracted by driving the main pump (6) and is transmitted to the linkage type extraction kettle group to perform supercritical extraction reaction;
the recovery system comprises a separation mechanism and a low-pressure balancing device (8), the separation mechanism is connected with the linkage type extraction kettle set and used for separating impurities from recovered carbon dioxide, and the low-pressure balancing device (8) is connected with the linkage type extraction kettle set and used for balancing the pressure in the extraction kettle during extraction reaction.
2. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: the first gas-liquid separator (3) comprises a tank body (9), a plurality of metal balls (10) arranged in the tank body (9) and heat exchange tubes (11) arranged on the periphery of the tank body (9), and a drain valve (12) is arranged at the bottom of the tank body (9).
3. The supercritical carbon dioxide extraction reaction system according to claim 2, wherein: the heat exchange tube (11) is provided with an upper connector and a lower connector, and the upper connector and the lower connector are communicated with the shell pass of the condenser (4).
4. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: linkage type extraction cauldron group includes first extraction cauldron (13), second extraction cauldron (14) and third extraction cauldron (15), the input of first extraction cauldron (13), second extraction cauldron (14) and third extraction cauldron (15) with all be equipped with the connecting pipe between the output of clarifier (7), and, the output of first extraction cauldron (13) with be equipped with the connecting pipe between the input of second extraction cauldron (14), the output of second extraction cauldron (14) with be equipped with the connecting pipe between the input of third extraction cauldron (15), the output of third extraction cauldron (15) with be equipped with the connecting pipe between the input of first extraction cauldron (13).
5. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: the output end of the condenser (4) is connected with a second liquid carbon dioxide storage tank (16), and the second liquid carbon dioxide storage tank (16) is connected with the linkage type extraction kettle set through an auxiliary pump (17).
6. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: the separation mechanism comprises a first heat exchanger (18), a second heat exchanger (19), a first-stage separation kettle (20) and a second-stage separation kettle (21), wherein the first heat exchanger (18), the first-stage separation kettle (20), the second heat exchanger (19) and the second-stage separation kettle (21) are sequentially connected in series.
7. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: the output ends of the first extraction kettle (13), the second extraction kettle (14) and the third extraction kettle (15) are all provided with an A interface.
8. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: the recovery system is further provided with a second gas-liquid separator (22) and a recovery tank (23), the input end of the second gas-liquid separator (22) is connected with the interface A, the output end of the second gas-liquid separator is connected with the input end of the low-pressure balancing device (8), and the recovery tank (23) is connected with the low-pressure balancing device (8) and the output end of the separation mechanism.
9. The supercritical carbon dioxide extraction reaction system according to claim 1, wherein: a metal rotor flowmeter (24) is arranged between the separation mechanism and the recovery tank (23).
CN202011416796.0A 2020-12-07 2020-12-07 Supercritical carbon dioxide extraction reaction system Pending CN112473169A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114085707A (en) * 2021-11-30 2022-02-25 唐川 Supercritical carbon dioxide extraction system of walnut oil
CN115501644A (en) * 2022-10-13 2022-12-23 西安科技大学 Circulating supercritical carbon dioxide-based coal decomposition promoting device and method

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Publication number Priority date Publication date Assignee Title
CN102210970A (en) * 2011-04-27 2011-10-12 李伟东 Desulfurization recycle unit for flue gas sulfur dioxide
CN110217794A (en) * 2019-05-09 2019-09-10 上海启元空分技术发展股份有限公司 A kind of production method and its process units of high-purity carbon dioxide
CN209475639U (en) * 2018-12-20 2019-10-11 华侨大学 A kind of supercritical extraction unit
CN110368713A (en) * 2019-08-22 2019-10-25 青岛利和萃取股份有限公司 One kind ten thousand upgrades supercritical carbon dioxide extraction system
CN210356072U (en) * 2019-06-24 2020-04-21 杭州一川新材料有限公司 Rectifying tower for separating product silane coupling agent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102210970A (en) * 2011-04-27 2011-10-12 李伟东 Desulfurization recycle unit for flue gas sulfur dioxide
CN209475639U (en) * 2018-12-20 2019-10-11 华侨大学 A kind of supercritical extraction unit
CN110217794A (en) * 2019-05-09 2019-09-10 上海启元空分技术发展股份有限公司 A kind of production method and its process units of high-purity carbon dioxide
CN210356072U (en) * 2019-06-24 2020-04-21 杭州一川新材料有限公司 Rectifying tower for separating product silane coupling agent
CN110368713A (en) * 2019-08-22 2019-10-25 青岛利和萃取股份有限公司 One kind ten thousand upgrades supercritical carbon dioxide extraction system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114085707A (en) * 2021-11-30 2022-02-25 唐川 Supercritical carbon dioxide extraction system of walnut oil
CN115501644A (en) * 2022-10-13 2022-12-23 西安科技大学 Circulating supercritical carbon dioxide-based coal decomposition promoting device and method

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Application publication date: 20210312