CN110393945B - Multichannel pressurized extraction flow path and extraction method thereof - Google Patents
Multichannel pressurized extraction flow path and extraction method thereof Download PDFInfo
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- CN110393945B CN110393945B CN201910833904.5A CN201910833904A CN110393945B CN 110393945 B CN110393945 B CN 110393945B CN 201910833904 A CN201910833904 A CN 201910833904A CN 110393945 B CN110393945 B CN 110393945B
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- 238000000605 extraction Methods 0.000 title claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000009826 distribution Methods 0.000 claims abstract description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 239000002699 waste material Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Classifications
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a multichannel pressurized extraction flow path, which comprises a multichannel high-pressure distribution flow path, an inlet valve, an outlet valve, a reaction kettle, a condenser, a collector, a nitrogen channel and a waste discharge tank, wherein the multichannel high-pressure distribution flow path is connected with the reaction kettle through the inlet valve; the inlet valve and the outlet valve adopt two-to-six-way valves, the inlet valve comprises a first gear, a second gear and a third gear, and the outlet valve comprises a first gear, a second gear and a third gear. The scheme utilizes a special flow path structure to enable the sample to generate efficient reaction, in particular to directly extract required elements from the solid sample, and also provides an extraction method of the multi-channel pressurized extraction flow path, which realizes rapid and automatic extraction.
Description
Technical Field
The invention relates to the field of experimental detection, in particular to a multichannel pressurized extraction flow path and an extraction method thereof.
Background
The existing extraction technology realizes extraction through a special extraction column, but the extraction column is prepared through the processes of activation, sample loading, leaching, blow-drying, elution and the like, the process is complex and consumes a great deal of time, and particularly when solid samples such as soil and the like are encountered, the extraction column is required to be homogenized or digested before being put on a machine for extraction. Extraction, while a well known process technology, remains a long felt need for more comprehensive extraction techniques for most laboratories, factories, etc.
Disclosure of Invention
The invention aims to provide a multichannel pressurized extraction flow path, which utilizes a special flow path structure to enable a sample to generate efficient reaction, in particular to directly extract required elements from a solid sample, has wide application prospect, and also provides an extraction method of the multichannel pressurized extraction flow path, so as to realize rapid and automatic extraction.
In order to achieve the above object, the technical scheme of the present invention is as follows:
the multichannel pressurized extraction flow path comprises a multichannel high-pressure distribution flow path, an inlet valve, an outlet valve, a reaction kettle, a condenser, a collector, a nitrogen channel and a waste discharge tank, wherein the multichannel high-pressure distribution flow path is connected with an inlet of the reaction kettle through the inlet valve; the inlet valve adopts a two-to-six-way valve, and comprises a first gear, a second gear and a third gear, wherein the first gear controls the opening between the multi-channel high-pressure distribution flow path and the reaction kettle flow path, the second gear controls the closing between the multi-channel high-pressure distribution flow path and the reaction kettle flow path, the third gear controls the closing between the multi-channel high-pressure distribution flow path and the reaction kettle flow path and enables the nitrogen channel to be connected with the reaction kettle; the outlet valve adopts a two-to-six-way valve, and comprises a first gear, a second gear and a third gear, wherein the first gear controls the opening between the condenser and the collector flow path, the second gear controls the closing between the condenser and the collector flow path, and the third gear controls the closing between the condenser and the collector flow path and enables the condenser to be connected with the waste discharge tank.
Preferably, the multi-channel high-pressure distribution flow path comprises a distribution valve, a high-pressure pump and a multi-way device, wherein the distribution valve is connected with an inlet of the multi-way device through the high-pressure pump, and the solvent to be reacted is placed on the distribution valve and is respectively pumped into the inlet of the multi-way device through the high-pressure pump by the distribution valve; the outlet of the multi-way device is connected with the inlet of the reaction kettle through an inlet valve, and the inlet valve controls the opening or closing between the multi-way device and a flow path of the reaction kettle.
Preferably, the multiplexer is connected with an overpressure protection valve, so as to prevent the pressure in the flow path from being overpressurized due to the continuous pressure of the high-pressure pump.
Preferably, the nitrogen channel is provided with a pneumatic pressure sensor, a first electromagnetic valve and a second electromagnetic valve, and the two ends of the third gear of the inlet valve are respectively provided with the first electromagnetic valve and the second electromagnetic valve which are connected with the nitrogen channel in parallel; and the third gear of the inlet valve is used for connecting or disconnecting the first electromagnetic valve and the second electromagnetic valve to control the opening or closing between the reaction kettle and the nitrogen channel, and the pneumatic pressure sensor is arranged on the parallel circuit to measure the nitrogen pressure between the inlet valve and the outlet valve.
Preferably, the two ends of the waste discharge tank are connected to the two ends of the III gear of the outlet valve, and the opening or closing between the condenser and the waste discharge tank is controlled by controlling the connection or disconnection of the two ends of the III gear.
Preferably, the multichannel high-pressure distribution flow path and the reaction kettle are respectively connected with a pressure sensor.
Preferably, the reaction kettle is also internally provided with a filter element, so that substances after reaction in the reaction kettle can be directly filtered out of the reaction kettle through the filter element, and thus, a filter is not required to be additionally arranged, and the structure and the operation are simpler.
An extraction method of a multichannel pressurized extraction flow path, comprising the following steps:
s1, preparation: firstly, placing a sample into a reaction kettle, and covering a kettle cover, wherein at the moment, an inlet valve is in a third gear state, an outlet valve is in a second gear state, a flow path between the inlet valve and the outlet valve is in a sealing state, and at the moment, a nitrogen channel is connected with the reaction kettle to detect the air tightness between the inlet valve and the outlet valve;
s2, starting extraction: switching an inlet valve into a first gear state, pumping the solvent to be reacted into a reaction kettle respectively through a multi-channel high-pressure distribution flow path, starting heating by a heating device in the reaction kettle, continuously pressurizing the multi-channel high-pressure distribution flow path, enabling a sample and the solvent to react for a period of time under high temperature and high pressure conditions, and then entering a condenser for condensation;
s3, extraction is finished: then switching the inlet valve to a second gear state, switching the outlet valve to an I gear state, and pushing the sample in the condenser into the collector through outlet pressure relief;
s4, cleaning: and finally, changing the solvent to be reacted into a cleaning solution, repeating the operations of S1 and S2, switching the outlet valve to a III gear, and pushing the cleaning solution into a waste discharge tank through the pressure relief of the outlet, thereby completing the cleaning.
Preferably, the inlet valve is switched to a third gear state after collection, nitrogen is introduced, and the residual sample in the reaction kettle is pushed out to the collector.
After the scheme is adopted, the inlet valve and the outlet valve of the invention are two-to-six-way valves with consistent specifications, and the invention has the following gain effects by means of the structural characteristics of the two-to-six-way valves:
1. the method can realize the high-temperature and high-pressure state, and control the reaction environment of the reaction kettle by controlling the opening and closing of the inlet valve and the outlet valve, so that the sample can efficiently react to complete the efficient extraction function, the extraction purpose is realized by a simple method in a short time, the extraction function is automatically completed at one time, and particularly, the method can directly extract the required elements from the solid sample, and has wide application prospect.
2. The invention can control the flow path switching by controlling the inlet valve and the outlet valve, so that the invention has the functions of airtight detection and cleaning and has complete functions.
3. In addition, the inlet valve and the outlet valve adopt two-to-six-way valves with consistent specifications, other valves are not needed, unified production is facilitated, and cost is saved.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of step S1 according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of step S2 according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of step S3 according to an embodiment of the present invention;
fig. 5 is a schematic structural diagram of step S4 according to an embodiment of the present invention.
Reference numerals illustrate:
the multi-channel high-pressure distribution flow path 1, the distribution valve 11, the high-pressure pump 12, the multiplexer 13, the overpressure protection valve 131, the inlet valve 2, the first gear 21, the second gear 22, the third gear 23, the outlet valve 3, the first gear 31, the second gear 32, the third gear 33, the reaction kettle 4, the condenser 5, the collector 6, the nitrogen channel 7, the pneumatic pressure sensor 71, the first electromagnetic valve 72, the second electromagnetic valve 73, the waste discharge tank 8 and the pressure sensor 9.
Detailed Description
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
Referring to fig. 1, a multi-channel pressurized extraction flow path includes a multi-channel high-pressure distribution flow path 1, an inlet valve 2, an outlet valve 3, a reaction kettle 4, a condenser 5, a collector 6, a nitrogen channel 7 and a waste discharge tank 8, wherein the multi-channel high-pressure distribution flow path 1 is connected with an inlet of the reaction kettle 4 through the inlet valve 2, a solvent to be reacted is pumped into the inlet of the reaction kettle 4 from the multi-channel high-pressure distribution flow path 1, the inlet valve 2 controls the opening or closing of the flow paths from the multi-channel high-pressure distribution flow path 1 to the reaction kettle 4, a sample can be placed into the reaction kettle by opening a kettle cover of the reaction kettle 4, a heating device (not shown in the figure) is arranged in the reaction kettle 4, an outlet of the reaction kettle 4 is connected with the inlet of the condenser 5, an outlet of the condenser 5 is connected with the collector 6 through the outlet valve 3, and the outlet valve 3 controls the opening or closing of the flow paths from the condenser 5 to the collector 6; the inlet valve 2 adopts a two-to-six-way valve, the inlet valve 2 comprises a first gear 21, a second gear 22 and a third gear 23, the first gear 21 controls the opening between the multi-channel high-pressure distribution flow path 1 and the flow path of the reaction kettle 4, the second gear 22 controls the closing between the multi-channel high-pressure distribution flow path 1 and the flow path of the reaction kettle 4, the third gear 23 controls the closing between the multi-channel high-pressure distribution flow path 1 and the flow path of the reaction kettle 4 and enables the nitrogen channel 7 to be connected with the reaction kettle 4; the outlet valve 3 adopts a two-to-six-way valve, the outlet valve 3 comprises a first gear 31, a second gear 32 and a third gear 33, the first gear 31 controls the opening between the condenser 5 and the collector 6, the second gear 32 controls the closing between the condenser 5 and the collector 6, the third gear 33 controls the closing between the condenser 5 and the collector 6, and the condenser 5 is connected with the waste discharge tank 8.
In order to specifically refine the structure of the multi-channel high-pressure distribution flow path 1, the multi-channel high-pressure distribution flow path 1 in the embodiment comprises a distribution valve 11, a high-pressure pump 12 and a multiplexer 13, wherein the distribution valve 11 is connected with the inlet of the multiplexer 13 through the high-pressure pump 12, and a solvent to be reacted is placed on the distribution valve 11 and is pumped into the inlet of the multiplexer 13 through the high-pressure pump 12 by the distribution valve; the outlet of the multiplexer 13 is connected with the inlet of the reaction kettle 4 through an inlet valve 2, and the inlet valve 2 controls the opening or closing of the flow path from the multiplexer 13 to the reaction kettle 4. As a preferred embodiment of the present case, the multiplexer 13 is connected to an overpressure protection valve 131, and the overpressure protection valve 131 can prevent the pressure in the flow path from being overpressurized by the continuous pressure of the high-pressure pump 12.
The nitrogen channel 7 is connected with the reaction kettle 4, in the preferred embodiment, a pneumatic pressure sensor 71, a first electromagnetic valve 72 and a second electromagnetic valve 73 are arranged on the nitrogen channel 7, a first electromagnetic valve 72 and a second electromagnetic valve 73 are respectively arranged at two ends of a third gear 23 of the inlet valve, and the first electromagnetic valve 72 and the second electromagnetic valve 73 are connected with the nitrogen channel 7 in parallel; the third gear 23 of the inlet valve is used for connecting or disconnecting the first electromagnetic valve 72 and the second electromagnetic valve 73 to control the opening or closing between the reaction kettle 4 and the nitrogen channel 7, and the pneumatic pressure sensor 71 is arranged on a parallel circuit to measure the nitrogen pressure between the inlet valve 2 and the outlet valve 3.
The third gear 33 controls the closing of the flow paths from the condenser 5 to the collector 6 and connects the condenser 5 to the waste tank 8, in this embodiment, the structure of the waste tank 8 is specifically refined, two ends of the waste tank 8 are connected to two ends of the third gear 33 of the outlet valve, and the opening or closing between the condenser 5 and the waste tank 8 is controlled by controlling the connection or disconnection of the two ends of the third gear 33.
In this embodiment, the invention also discloses an extraction method of the multi-channel pressurized extraction flow path, which comprises the following steps:
s1, preparation: as shown in fig. 2, a sample is put into a reaction kettle 4, a kettle cover is covered, at this time, an inlet valve 2 is in a third gear 23 state, an outlet valve 3 is in a second gear 32 state, a flow path between the inlet valve 2 and the outlet valve 3 is in a sealing state, and at this time, a nitrogen channel 7 is connected with the reaction kettle 4 to detect the air tightness between the inlet valve 2 and the outlet valve 3;
s2, starting extraction: as shown in fig. 3, after the air tightness detection is finished, the inlet valve 2 is switched to a first gear 21 state, the outlet valve 3 is still in a second gear 32 state, then the solvent to be reacted is placed in the distribution valve 11 and is pumped into the inlets of the multipass devices 13 through the high-pressure pump 12 respectively by the distribution valve, the solvent enters the reaction kettle 4 through the outlets of the multipass devices 13, the heating device in the reaction kettle 4 starts to heat according to the set temperature of the sample requirement, the high-pressure pump 12 continuously pressurizes according to the set pressure of the sample requirement, so that the sample and the solvent react for a period of time under the high-temperature high-pressure condition, and then enter the condenser 5 from the outlet of the reaction kettle 4 to be condensed, and the reaction time is set according to the set time of the sample requirement;
s3, extraction is finished: as shown in fig. 4, the inlet valve 2 is then switched to the second gear 22 state, the outlet valve 3 is switched to the i gear 31 state, and the sample in the condenser 5 is pushed into the collector 6 through the outlet pressure relief;
further, the inlet valve 2 is switched to a third gear 23 state after collection, nitrogen is introduced, a sample remained in the reaction kettle 4 is pushed out to the collector 6, and nitrogen blowing concentration effect can be achieved in the collector 6 by continuously blowing nitrogen.
S4, cleaning: as shown in fig. 5, finally, the solvent to be reacted is changed into a cleaning solution, and after repeating the operations of S1 and S2, the outlet valve 3 is switched to the iii gear 33, and the cleaning solution is pushed into the waste discharge tank 8 through the outlet pressure relief, thus the cleaning can be completed. In this embodiment, the reaction kettle 4 is further provided with a filter element (not shown in the figure), so that the substances reacted in the reaction kettle 4 can be directly filtered out of the reaction kettle 4 through the filter element, and thus, no additional filter is needed, and the structure and operation are simpler.
In this embodiment, the multichannel high-pressure distribution flow path 1 and the reaction kettle 4 are respectively connected with a pressure sensor 9, so that the pressure condition in the reaction kettle 4 can be known in real time.
The device has the advantages that the two-to-six-way valve is adopted to simultaneously perform the extraction operation of two samples, so that the extraction process of a plurality of samples is accelerated.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A multi-channel pressurized extraction flow path, characterized by: the reaction kettle comprises a multichannel high-pressure distribution flow path, an inlet valve, an outlet valve, a reaction kettle, a condenser, a collector, a nitrogen channel and a waste discharge tank, wherein the multichannel high-pressure distribution flow path is connected with an inlet of the reaction kettle through the inlet valve; the inlet valve adopts a two-to-six-way valve, and comprises a first gear, a second gear and a third gear, wherein the first gear controls the opening between the multi-channel high-pressure distribution flow path and the reaction kettle flow path, the second gear controls the closing between the multi-channel high-pressure distribution flow path and the reaction kettle flow path, the third gear controls the closing between the multi-channel high-pressure distribution flow path and the reaction kettle flow path and enables the nitrogen channel to be connected with the reaction kettle; the outlet valve adopts a two-to-six-way valve, and comprises a first gear, a second gear and a third gear, wherein the first gear controls the opening between the condenser and the collector flow path, the second gear controls the closing between the condenser and the collector flow path, and the third gear controls the closing between the condenser and the collector flow path and enables the condenser to be connected with the waste discharge tank;
the multichannel high-pressure distribution flow path comprises a distribution valve, a high-pressure pump and a multipass device, wherein the distribution valve is connected with an inlet of the multipass device through the high-pressure pump, and a solvent to be reacted is placed in the distribution valve and is pumped into the inlet of the multipass device through the high-pressure pump by the distribution valve; the outlet of the multi-way device is connected with the inlet of the reaction kettle through an inlet valve, and the inlet valve controls the opening or closing between the multi-way device and a flow path of the reaction kettle;
the nitrogen channel is provided with a pneumatic pressure sensor, a first electromagnetic valve and a second electromagnetic valve, two ends of a third gear of the inlet valve are respectively provided with the first electromagnetic valve and the second electromagnetic valve, and the first electromagnetic valve and the second electromagnetic valve are connected with the nitrogen channel in parallel; the third gear of the inlet valve is used for connecting or disconnecting the first electromagnetic valve and the second electromagnetic valve to control the opening or closing between the reaction kettle and the nitrogen channel, and the pneumatic pressure sensor is arranged on the parallel circuit to measure the nitrogen pressure between the inlet valve and the outlet valve;
the two ends of the waste discharge tank are connected to the two ends of the III gear of the outlet valve, and the opening or closing between the condenser and the waste discharge tank is controlled by controlling the connection or disconnection of the two ends of the III gear;
the multichannel high-pressure distribution flow path and the reaction kettle are respectively connected with a pressure sensor.
2. The multi-channel pressurized extraction flow path of claim 1, wherein: the multipass device is connected with an overpressure protection valve.
3. The multi-channel pressurized extraction flow path of claim 1, wherein: and a filter element is also arranged in the reaction kettle.
4. An extraction method of a multichannel pressurized extraction flow path is characterized by comprising the following steps of: a multi-channel pressurized extraction flow path as claimed in any one of claims 1 to 3, the method comprising the steps of:
s1, preparation: firstly, placing a sample into a reaction kettle, and covering a kettle cover, wherein at the moment, an inlet valve is in a third gear state, an outlet valve is in a second gear state, a flow path between the inlet valve and the outlet valve is in a sealing state, and at the moment, an airtight detection device is connected with the reaction kettle to detect the airtight property between the inlet valve and the outlet valve;
s2, starting extraction: switching an inlet valve into a first gear state, pumping the solvent to be reacted into a reaction kettle respectively through a multi-channel high-pressure distribution flow path, starting heating by a heating device in the reaction kettle, continuously pressurizing the multi-channel high-pressure distribution flow path, enabling a sample and the solvent to react for a period of time under high temperature and high pressure conditions, and then entering a condenser for condensation;
s3, extraction is finished: then switching the inlet valve to a second gear state, switching the outlet valve to an I gear state, and pushing the sample in the condenser into the collector through outlet pressure relief;
s4, cleaning: and finally, changing the solvent to be reacted into a cleaning solution, repeating the operations of S1 and S2, switching the outlet valve to a III gear, and pushing the cleaning solution into a waste discharge tank through the pressure relief of the outlet, thereby completing the cleaning.
5. The method according to claim 4, wherein: s3, switching the inlet valve to a third gear state after collection, introducing nitrogen, and pushing out the residual sample in the reaction kettle to the collector.
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| WO2021227546A1 (en) * | 2020-05-12 | 2021-11-18 | 睿科集团(厦门)股份有限公司 | Multifunctional sample extraction flow path and method |
| CN112858598B (en) * | 2021-01-05 | 2022-10-18 | 北京优兴科仪科技开发有限公司 | Pesticide residue detector |
| CN114159827A (en) * | 2021-11-30 | 2022-03-11 | 李志军 | Supercritical CO of green tea2Extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT411154B (en) * | 2002-01-17 | 2003-10-27 | Wolfsbauer Barbara | Process and dual pressure assembly to extract volatile substances from crushed solids |
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| JPH01221660A (en) * | 1988-03-01 | 1989-09-05 | Japan Spectroscopic Co | Extraction chromatograph separator |
| CN1528487A (en) * | 2003-10-10 | 2004-09-15 | 大连理工大学 | Basic process flow of semicontinuous supercritical fluid extraction |
| CN102445503A (en) * | 2011-09-22 | 2012-05-09 | 中国海洋大学 | Combined analytic device for subcritical fluid extraction-liquid chromatography (LC) |
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