CN115155099A - Flow path of multi-channel pressure solvent extraction instrument system and application method - Google Patents

Flow path of multi-channel pressure solvent extraction instrument system and application method Download PDF

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CN115155099A
CN115155099A CN202210716018.6A CN202210716018A CN115155099A CN 115155099 A CN115155099 A CN 115155099A CN 202210716018 A CN202210716018 A CN 202210716018A CN 115155099 A CN115155099 A CN 115155099A
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pressure
extraction
pipeline
valve
extraction tank
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刘永利
朱苗苗
徐加乐
李全伟
韩磊磊
谢新刚
邓宛梅
胡克
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Beijing Labtech Instruments Co ltd
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Beijing Labtech Instruments Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • 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
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0207Control systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0215Solid material in other stationary receptacles
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction

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  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
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  • Automation & Control Theory (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention provides a flow path of a multi-channel pressure solvent extraction instrument system and an application method, which are characterized in that: the system comprises a gas-liquid supply unit, a flow path distribution unit, a heating sealing unit, a collection unit, a flow path distribution unit, a flow path control unit, a control unit and a control unit, wherein the gas-liquid supply unit is connected with the heating sealing unit through a pipeline, the bottom end of the heating sealing unit is connected with the top end of the collection unit through a pipeline, and the full-automatic treatment such as sealing, heating, boosting, static extraction, purging, automatic collection and the like can be carried out during sample extraction.

Description

Flow path of multi-channel pressure solvent extraction instrument system and application method
Technical Field
The invention relates to a flow path of a multi-channel pressure solvent extraction instrument system and an application method thereof.
Background
Pressure solvent extraction, or rapid solvent extraction, is a sample pretreatment technique developed in recent years for solid/semisolid extraction. Compared with the traditional extraction technology, the extraction technology can extract samples at higher temperature and pressure, has the advantages of small amount of organic solvent, high extraction speed, high sample recovery rate and the like, and is widely applied to the fields of environment, agriculture, food safety and the like. The high-pressure liquid in the rapid solvent extraction is conveyed by using a cam infusion pump as liquid conveying power.
With the widespread use of solvent extraction techniques, there are several systematic problems arising from the different sample matrices and the different purposes of application.
On one hand, in the process of batching samples, the existing multi-channel system cannot control the extraction of a single sample, when the number of samples does not meet the loading capacity of the lowest sample, an extraction tank which is not filled with the samples is usually required to be selected as an assistant, so that the use experience is reduced, and meanwhile, the cost in the aspects of solvents, consumables, later cleaning and the like is increased. In the closest technology, a two-to-six-way valve is adopted as a flow path high-pressure valve, so that the working positions of two channels can be controlled simultaneously, but the control of a single channel cannot be met.
On the other hand, in the automatic treatment process, the solvent needs to be emptied to the system when the system is reused due to factors such as temperature, solvent mixing, solvent replacement, long-time non-use and the like, so that the operation preparation time of personnel and the waste of the solvent are increased, and the cost is further increased.
Meanwhile, the existing system is not provided with a design for preventing the cross among channels, so that the problem of cross contamination among samples is easily caused.
Furthermore, based on the research field, the development work of a new method is usually required to be carried out by comparing cross experiments, and at this time, two key influencing factors of temperature and pressure are required to have higher control precision, and the high-precision range control of the two factors, especially the pressure factor, cannot be carried out in the prior art.
In addition, in the environmental analysis, oil samples, the field of traditional Chinese medicine and other application fields are individual, the high viscosity of the sample is one of the reasons for limiting the use of the pressure solvent, and the samples containing components such as oil, plastic and the like usually cause pipeline blockage, so that the pressure solvent extraction cannot be well applied.
In addition, the existing pressure boosting technology adopts a large flow rate pressure boosting or gradient pressure boosting mode to input the solvent, the former can shorten the experimental time, but pressure overshoot is easily caused; the latter target pressure temperature, but with low efficiency.
Disclosure of Invention
The invention provides a flow path of a multi-channel pressure solvent extraction instrument system and an application method thereof, which solve the problem of extraction of a single sample, the problem of experiment interruption caused by generation of solvent bubbles, the problem of easy cross contamination in the experiment process, the problems that the original mode is single in working mode and cannot be applied to various fields and applications, the problem that blockage is easy to occur in the experiment process of special samples, the flow extraction working mode of system improvement and initiation, and the problem that pressure overshoot or experiment time consumption is easy to cause in a boosting mode.
In order to achieve the purpose, the invention adopts the technical scheme that:
a multichannel pressure solvent extraction appearance system flow path which characterized in that: the gas-liquid supply unit is connected with a heating sealing unit through a pipeline of a flow path distribution unit, and the bottom end of the heating sealing unit is connected with a top end pipeline of the collection unit;
the gas-liquid supply unit is internally provided with a gas source and a plurality of solvent bottles respectively, the gas source is connected with a medium valve pipeline, each solvent bottle is connected with a proportional valve pipeline correspondingly arranged, the proportional valves are connected with a mixer pipeline respectively, the mixer is connected with the medium valve pipeline, a composite emptying valve and an infusion pump are sequentially arranged between the medium valve and the mixer, and the medium valve is also connected with a total pressure sensor pipeline;
a distributor is arranged in the flow path distribution unit, the top end of the distributor is connected with the total pressure sensor through a pipeline, the bottom end of the distributor is respectively connected with a plurality of upper sealing valve through pipelines, the inlet end of each upper sealing valve is respectively provided with a one-way valve, and the outlet end of each upper sealing valve is respectively provided with a channel pressure sensor;
a heating body is arranged in the heating sealing unit, the heating body can move back and forth through a slide rail, a plurality of extraction tanks are placed on the heating body, a plurality of upper sealing seats and lower sealing seats are arranged in the heating sealing unit, each upper sealing seat is respectively connected with the corresponding channel pressure sensor pipeline and forms an independent passage, a sealing mechanism is arranged in the heating sealing unit, the sealing mechanism is in transmission connection with the upper sealing seats, the sealing mechanism can control the upper sealing seats to move downwards and drive the heating body to move downwards to a sealing position, and the upper sealing seats and the lower sealing seats respectively contact and seal the top ends and the bottom ends of the extraction tanks;
the waste collection device is characterized in that a plurality of lower sealing valves are arranged in the collection unit, the top ends of the lower sealing valves are respectively connected with the corresponding lower sealing seat pipelines to form independent passages, the bottom ends of the lower sealing valves are respectively communicated with the corresponding heating collection pipelines, a plurality of waste discharge pipelines are arranged in the collection unit, each waste discharge pipeline is respectively connected with a waste discharge concentrated block pipeline, a collection assembly and a collection mechanism are arranged in the collection unit, the collection mechanism is in transmission connection with the collection assembly, and the collection mechanism can drive the collection assembly to move up and down and is communicated with the heating collection pipelines and the waste discharge pipelines.
The multichannel pressure solvent extraction appearance system flow path, wherein: the proportional valve adjusts the mixing proportion of the solvent by controlling the opening and closing time, and the medium valve can be switched into three states, namely pipeline closing, gas pipeline communication and liquid pipeline communication.
The multichannel pressure solvent extraction appearance system flow path, wherein: and the upper sealing seat is provided with a manual plug valve, so that the pressure can be manually relieved.
The multichannel pressure solvent extraction appearance system flow path, wherein: the end of heating collection pipeline sets up collects the needle, the end of exhaust pipeline sets up the waste gas needle, place a plurality of receiving flask in the collection subassembly, the rising of collection subassembly removes the confession the collection needle reaches the waste gas needle pierces through the top seal pad of receiving flask.
An application method of a flow path of a multi-channel pressure solvent extraction instrument system is characterized by comprising the following steps:
the method comprises the following steps that 1, a test process is placed, a sample is placed in an extraction tank and placed on a heating body, an upper sealing seat is controlled by a sealing mechanism to move downwards, the upper sealing seat moves downwards together with the extraction tank by pressing down the heating body, the bottom end of the extraction tank moves to a lower sealing seat, at the moment, the upper sealing seat and the lower sealing seat respectively contact and seal the top end and the bottom end of the extraction tank, a collection mechanism drives a collection assembly and a collection bottle to move upwards together, and a top sealing gasket of the collection bottle is respectively penetrated by a collection needle and an exhaust gas needle;
step 2, closing a lower sealing valve, opening an upper sealing valve, adjusting a medium valve from a closed pipeline state to a gas pipeline open state, and enabling the medium valve to be in a communication state with a gas source, opening the gas source and temporarily inflating the extraction tank, closing the upper sealing valve, comparing the recorded values of the total pressure sensor and the channel pressure sensors, determining that the placement position of the extraction tank is correct if the recorded values are within a specified range, otherwise, determining that the placement position of the extraction tank is incorrect, and readjusting the placement position of the extraction tank until the recorded values are correct;
step 3, a heating process, namely, the upper sealing valve is opened again, the heating body starts to heat, the medium valve is adjusted to be in a liquid pipeline communication state from a gas pipeline opening state, the infusion pump is opened, the flow rate of each solvent is further controlled by adjusting the opening time of the proportional valve, the purpose of adjusting the solvent ratio is achieved, each solvent flows into the mixer to be mixed to form a mixed solvent, and the mixed solvent is conveyed into the extraction tank through the infusion pump;
step 4, a boosting process, wherein the boosting stage in the extraction tank is divided into two stages, namely a pre-full pressure stage and a method pressure stage, the pre-full pressure stage is to preheat the extraction tank through the heating body, so that the normal-temperature mixed solvent injected into the extraction tank can be preheated, certain pressure can be released in the preheating process, the preheating can enable the pressure in the static extraction stage to be more stable, if the pre-full pressure stage is not carried out, the method pressure is directly set, the pressure in the extraction tank is enabled to reach the method set pressure in advance, the boosting process adopts a PID program to boost, and the boosting efficiency and accuracy in the stage are ensured;
if the pressure does not rise within a certain time in the boosting process, the composite emptying valve is opened to empty the gas or bubbles in the liquid pipeline, the composite emptying valve is closed, and the infusion pump continues to inject, mix and dissolve the gas or bubbles into the extraction tank;
step 5, an extraction process, wherein the temperature of the extraction tank is raised to the method temperature by the heating body, and when the pressure is raised to the method pressure, the infusion pump, the medium valve and the upper sealing valve are closed, the mixed solvent in the extraction tank is kept at the method temperature and the method pressure, and then the extraction process enters a static extraction stage;
the static extraction stage is divided into three modes of standard extraction, constant pressure extraction and flow extraction;
in a standard extraction mode, the pressure rise and the pressure drop in the extraction tank are not processed, the extraction efficiency generally depends on the temperature rather than the pressure, and the change of the pressure has little influence on the extraction result;
in a constant pressure extraction mode, the pressure of each channel is monitored through the whole process of each channel pressure sensor, and pressure compensation or pressure relief is carried out after the pressure abnormality of the extraction tank of the corresponding channel exceeds a certain range;
in the pressure supplementing process, the upper sealing valve of the corresponding channel is opened, the infusion pump is started, mixed solvent is injected into the extraction tank needing pressure supplementing, and the infusion pump and the upper sealing valve of the corresponding channel are closed until the static extraction process is finished after the pressure in the extraction tank with abnormal pressure is recovered to the method pressure;
in the pressure relief process, the lower sealing valve of the corresponding channel is slowly opened, so that the extracting solution in the extracting tank needing pressure relief flows into the corresponding collecting bottle in the collecting assembly through the lower sealing valve, meanwhile, the pressure in the channel is judged in real time through the channel pressure sensor, and when the pressure is relieved to the method pressure, the lower sealing valve is quickly closed until the static extracting process is finished;
in a flowing extraction mode, after entering a static extraction flow, opening each lower sealing valve to a certain extent, monitoring the channel pressure sensor to know that the pressure in each extraction tank is reduced in a small extent, at the moment, stopping the opening of the lower sealing valve, and keeping the existing state, meanwhile, as the method in the pressure supplementing process, starting the infusion pump, continuously injecting a mixed solvent into the extraction tank needing pressure supplementing, and simultaneously continuously flowing the extracting solution in the extraction tank into the corresponding collecting bottle in the collecting assembly, so that the pressure in the extraction tank can be kept in a method pressure range until the static extraction flow is finished;
step 6, a collecting process is performed, wherein the upper sealing valve and the lower sealing valve are opened, the extracting solution flows into the collecting bottle by using the pressure in the extracting tank, the collecting process is finished after the pressure is sensed to be reduced to a set value by the channel pressure sensor, and the heating collecting pipeline is always in an open state in the collecting process, so that the extracting solution can be kept in a range of a set temperature in the heating collecting pipeline, and the extracting solution containing grease or other extracting solutions which are easy to condense due to the reduction of temperature and pressure is prevented from blocking the pipeline;
and 7, a flushing process, namely opening the upper sealing valve, the lower sealing valve and the infusion pump, cleaning the extraction tank and the pipeline through the infusion pump, then entering a purging process, performing gas purging on the extraction tank and the pipeline by using the gas source, allowing waste liquid and waste gas generated by flushing and purging to enter the collecting bottle, and discharging the waste gas outwards through the waste discharge pipeline and the waste discharge concentration block.
The invention has the beneficial effects that: the problem of extract single sample is solved, the problem that causes the experiment interrupt because of the production of solvent bubble has been solved, the problem of easily producing cross contamination in the experimentation has been solved, the problem that original mode working method is single, can not be suitable for multiple fields and application has been solved, the problem that easily takes place to block up in the special sample experimentation has been solved, the flow of system improvement and initiation draws the working method, the problem that the mode of stepping up easily causes pressure to overshoot or experiment length consuming time has been solved.
Drawings
FIG. 1 is a schematic diagram of the flow path of a multi-channel pressure solvent extractor system.
Description of reference numerals: 1-a gas-liquid supply unit; 2-a flow path distribution unit; 3-heating the sealing unit; 4-a collection unit; 101-solvent bottle; 102-a proportional valve; 103-a mixer; 104-an infusion pump; 105-a compound evacuation valve; 106-a media valve; 107-gas source; 108-total pressure sensor; 109-safety valve; 201-a dispenser; 202-a one-way valve; 203-upper sealing valve; 204-channel pressure sensor; 301-upper seal mount; 302-manual plug valve; 303-a heating body; 304-an extraction tank; 305-lower seal seat; 306-a sealing mechanism; 401-lower sealing valve; 402-a heating collection line; 403-a collection assembly; 404-a waste discharge pipeline; 405-waste discharge concentration block; 406-collection mechanism.
Detailed Description
As shown in FIG. 1, the present invention provides a flow path of a multi-channel pressure solvent extraction apparatus system, wherein a gas-liquid supply unit 1 is connected with a heating sealing unit 3 through a flow path distribution unit 2, and the bottom end of the heating sealing unit 3 is connected with the top end of a collection unit 4 through a pipeline.
The gas-liquid supply unit 1 is internally provided with a gas source 107 and a plurality of solvent bottles 101, the gas source 107 is connected with a medium valve 106 through a pipeline, each solvent bottle 101 is connected with a proportional valve 102 correspondingly arranged through a pipeline, the proportional valve 102 adjusts the mixing proportion of the solvents by controlling the opening and closing time, the proportional valve 102 is connected with a mixer 103 through a pipeline, the mixer 103 is connected with the medium valve 106 through a pipeline, the medium valve 106 can be switched into three states, namely pipeline closing, gas pipeline communication and liquid pipeline communication, a composite emptying valve 105 and an infusion pump 104 are sequentially arranged between the medium valve 106 and the mixer 103, and the medium valve 106 is further connected with a total pressure sensor 108 through a pipeline.
A distributor 201 is arranged in the flow path distribution unit 2, the top end of the distributor 201 is in pipeline connection with the total pressure sensor 108, the bottom end of the distributor 201 is in pipeline connection with a plurality of upper sealing valves 203, respectively, an inlet end of each upper sealing valve 203 is provided with a one-way valve 202, and an outlet end of each upper sealing valve 203 is provided with a channel pressure sensor 204.
A heating body 303 is arranged in the heating and sealing unit 3, the heating body 303 can move back and forth through a sliding rail, a plurality of extraction tanks 304 are placed on the heating body 303, a plurality of upper sealing seats 301 and lower sealing seats 305 are arranged in the heating and sealing unit 3, each upper sealing seat 301 is respectively connected with the corresponding channel pressure sensor 204 through a pipeline to form an independent passage, a manual plug valve 302 is arranged on each upper sealing seat 301 and can be manually decompressed, a sealing mechanism 306 is arranged in the heating and sealing unit 3, the sealing mechanism 306 is in transmission connection with the upper sealing seats 301, the sealing mechanism 306 can control the upper sealing seats 301 to move downwards and drive the heating body 303 to move downwards to a sealing position, and the upper sealing seats 301 and the lower sealing seats 305 respectively contact and seal the top ends and the bottom ends of the extraction tanks 304;
the waste collection device is characterized in that a plurality of lower sealing valves 401 are arranged in the collection unit 4, the top end of each lower sealing valve 401 is connected with the corresponding lower sealing seat 305 through a pipeline, an independent passage is formed, the bottom end of each lower sealing valve 401 is communicated with the corresponding heating collection pipeline 402, a plurality of waste discharge pipelines 404 are arranged in the collection unit 4, each waste discharge pipeline 404 is connected with a waste discharge concentration block 405 through a pipeline, a collection assembly 403 and a collection mechanism 406 are arranged in the collection unit 4, the collection mechanism 406 is in transmission connection with the collection assembly 403, the collection mechanism 406 can drive the collection assembly 403 to move up and down and is communicated with the heating collection pipeline 402 and the waste discharge pipeline 404, a collection needle is arranged at the tail end of the heating collection pipeline 402, a waste gas needle is arranged at the tail end of the waste discharge pipeline 404, a plurality of collection bottles are arranged in the collection assembly 403, and the collection assembly 403 moves up and penetrates through sealing gaskets at the top of the collection needles.
An application method of a flow path of a multi-channel pressure solvent extraction instrument system is characterized by comprising the following steps:
step 1, placing a test flow, wherein a sample is loaded into an extraction tank 304 and placed on a heating body 303, a sealing mechanism 306 controls an upper sealing seat 301 to move downwards, the upper sealing seat 301 moves downwards together by pressing the extraction tank 304 on the heating body 303, the bottom end of the extraction tank 304 moves to a lower sealing seat 305, at the moment, the upper sealing seat 301 and the lower sealing seat 305 respectively contact and seal the top end and the bottom end of the extraction tank 304, a collecting mechanism 406 drives a collecting assembly 403 and a collecting bottle to move upwards together, and a top sealing gasket of the collecting bottle is respectively pierced by a collecting needle and an exhaust gas needle;
step 2, closing the lower sealing valve 401, opening the upper sealing valve 203, adjusting the medium valve 106 from a closed pipeline state to a gas pipeline open state, and communicating with the gas source 107, opening the gas source 107 and charging the extraction tank 304 for a while, closing the upper sealing valve 203, comparing the recorded values of the total pressure sensor 108 and the channel pressure sensors 204, determining that the placement position of the extraction tank 304 is correct, and otherwise, determining that the placement position of the extraction tank 304 is incorrect, and readjusting the placement position of the extraction tank 304 until the placement position is correct;
step 3, a temperature rise process, in which the upper sealing valve 203 is opened again, the heating body 303 starts to heat, the medium valve 106 is adjusted from a gas pipeline opening state to a liquid pipeline communication state, the infusion pump 104 is opened, the proportional valve 102 adjusts the opening time to further control the flow rate of each solvent, so as to achieve the purpose of adjusting the solvent ratio, each solvent flows into the mixer 103 to be mixed to form a mixed solvent, and the mixed solvent is conveyed to the extraction tank 304 through the infusion pump 104;
step 4, a boosting process, wherein a boosting stage in the extraction tank 304 is divided into two stages, namely a pre-full pressure stage and a method pressure stage, the pre-full pressure stage is to preheat the extraction tank 304 through the heating body 303, so that the normal-temperature mixed solvent injected into the extraction tank 304 can be preheated, a certain pressure can be released in the preheating process, the preheating can make the pressure in the static extraction stage more stable, if the normal-temperature mixed solvent does not enter the method pressure stage directly without entering the pre-full pressure stage, the method is directly set for the pressure, the pressure in the extraction tank 304 is made to reach the method set pressure in advance, the boosting process adopts a PID program for boosting, and the boosting efficiency and accuracy of the stage are ensured;
if the pressure does not rise within a certain time in the boosting process, the composite emptying valve 105 is opened to empty the gas or bubbles in the liquid pipeline, the composite emptying valve (105) is closed, and the infusion pump 104 continues to inject, mix and dissolve the gas or bubbles into the extraction tank 304;
step 5, an extraction process, wherein the heating body 303 raises the temperature of the extraction tank 304 to a process temperature, and when the pressure is raised to a process pressure, the infusion pump 104, the medium valve 106 and the upper sealing valve 203 are closed, the mixed solvent in the extraction tank 304 is kept at the process temperature and the process pressure, and the static extraction stage is started;
the static extraction stage is divided into three modes of standard extraction, constant pressure extraction and flow extraction;
in the standard extraction mode, the pressure rise and the pressure drop in the extraction tank 304 are not processed, the extraction efficiency generally depends on the temperature rather than the pressure, and the change of the pressure has little influence on the extraction result;
in the constant-pressure extraction mode, the pressure of each channel is monitored through the whole process of each channel pressure sensor 204, and pressure compensation or pressure relief is carried out after the pressure abnormality of the extraction tank 304 of the corresponding channel exceeds a certain range;
in the pressure supplementing process, the upper sealing valve 203 of the corresponding channel is opened, the infusion pump 104 is opened, the mixed solvent is injected into the extraction tank 304 requiring pressure supplementing, and after the pressure in the extraction tank 304 with abnormal pressure is restored to the method pressure, the infusion pump 104 and the upper sealing valve 203 of the corresponding channel are closed until the static extraction process is finished;
in the pressure relief process, the lower sealing valve 401 of the corresponding channel is slowly opened, so that the extracting solution in the extraction tank 304, which needs to be depressurized, flows into the corresponding collection bottle in the collection assembly 403 through the lower sealing valve 401, meanwhile, the pressure in the channel is determined in real time through the channel pressure sensor 204, and when the pressure is relieved to the method pressure, the lower sealing valve 401 is quickly closed until the static extraction process is finished;
in the flow extraction mode, after entering the static extraction process, each lower sealing valve 401 is opened to a certain extent, the channel pressure sensor 204 is monitored to know that the pressure in each extraction tank 304 decreases to a small extent, at this time, the opening extent of the lower sealing valve 401 is stopped, and the existing state is maintained, meanwhile, as in the above-mentioned method in the pressure compensation process, the infusion pump 104 is opened, the mixed solvent is continuously injected into the extraction tank 304 requiring pressure compensation, the extraction liquid in the extraction tank 304 simultaneously and continuously flows into the corresponding collection bottle in the collection assembly 403, and the pressure in the extraction tank 304 can be maintained within the method pressure range until the static extraction process is finished;
step 6, a collecting process, in which the upper sealing valve 203 and the lower sealing valve 401 are opened, the extracting solution flows into the collecting bottle by using the pressure in the extraction tank 304, the collecting process is ended after the channel pressure sensor 204 senses that the pressure is reduced to a set value, and the heating and collecting pipeline 402 is always in an open state during the collecting process, so that the extracting solution can be kept in a set temperature range in the heating and collecting pipeline 402, and the extracting solution containing grease or other extracting solutions which are easy to be condensed due to the reduction of temperature and pressure is prevented from blocking the pipeline;
step 7, a flushing process, in which the upper sealing valve 203, the lower sealing valve 401 and the infusion pump 104 are opened, the extraction tank 304 and the pipeline are cleaned by the infusion pump 104, then the process enters a purging process, the extraction tank 304 and the pipeline are purged by gas by using the gas source 107, waste liquid and waste gas generated by flushing and purging enter the collecting bottle, and the waste gas is discharged outwards through the waste discharge pipeline 404 and the waste discharge concentration block 405.
The invention has the advantages that:
the problem of extract single sample is solved, the problem that causes the experiment interrupt because of the production of solvent bubble has been solved, the problem of easily producing cross contamination in the experimentation has been solved, the problem that original mode working method is single, can not be suitable for multiple fields and application has been solved, the problem that easily takes place to block up in the special sample experimentation has been solved, the flow of system improvement and initiation draws the working method, the problem that the mode of stepping up easily causes pressure to overshoot or experiment length consuming time has been solved.
The foregoing description is intended to be illustrative rather than limiting, and it will be appreciated by those skilled in the art that many modifications, variations or equivalents may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (5)

1. A multichannel pressure solvent extraction appearance system flow path which characterized in that: the gas-liquid supply unit (1) is connected with the heating sealing unit (3) through a pipeline of the flow path distribution unit (2), and the bottom end of the heating sealing unit (3) is connected with the top end pipeline of the collection unit (4);
the gas-liquid supply unit (1) is internally provided with a gas source (107) and a plurality of solvent bottles (101) respectively, the gas source (107) is connected with a medium valve (106) through a pipeline, each solvent bottle (101) is connected with a corresponding proportional valve (102) through a pipeline, the proportional valves (102) are connected with a mixer (103) through pipelines, the mixer (103) is connected with the medium valve (106) through a pipeline, a composite emptying valve (105) and an infusion pump (104) are sequentially arranged between the medium valve (106) and the mixer (103), and the medium valve (106) is further connected with a total pressure sensor (108) through a pipeline;
a distributor (201) is arranged in the flow path distribution unit (2), the top end of the distributor (201) is in pipeline connection with the total pressure sensor (108), the bottom end of the distributor (201) is in pipeline connection with a plurality of upper sealing valves (203) respectively, the inlet end of each upper sealing valve (203) is provided with a one-way valve (202), and the outlet end of each upper sealing valve (203) is provided with a channel pressure sensor (204);
a heating body (303) is arranged in the heating sealing unit (3), the heating body (303) can move back and forth through a sliding rail, a plurality of extraction tanks (304) are placed on the heating body (303), a plurality of upper sealing seats (301) and lower sealing seats (305) are arranged in the heating sealing unit (3), each upper sealing seat (301) is respectively connected with the corresponding channel pressure sensor (204) through a pipeline and forms an independent passage, a sealing mechanism (306) is arranged in the heating sealing unit (3), the sealing mechanism (306) is in transmission connection with the upper sealing seats (301), the sealing mechanism (306) can control the upper sealing seats (301) to move downwards and drive the heating body (303) to move downwards to a sealing position, and the upper sealing seats (301) and the lower sealing seats (305) respectively contact and seal the top ends and the bottom ends of the extraction tanks (304);
the waste collection device is characterized in that a plurality of lower sealing valves (401) are arranged in the collection unit (4), the top ends of the lower sealing valves (401) are respectively connected with the corresponding lower sealing seats (305) through pipelines to form independent passages, the bottom ends of the lower sealing valves (401) are respectively communicated with the corresponding heating collection pipelines (402), a plurality of waste discharge pipelines (404) are arranged in the collection unit (4), each waste discharge pipeline (404) is respectively connected with a waste discharge concentration block (405) through a pipeline, a collection assembly (403) and a collection mechanism (406) are arranged in the collection unit (4), the collection mechanism (406) is in transmission connection with the collection assembly (403), and the collection mechanism (406) can drive the collection assembly (403) to move up and down and is communicated with the heating collection pipelines (402) and the waste discharge pipelines (404).
2. The multi-channel pressure solvent extractor system flow path of claim 1, wherein: the proportional valve (102) adjusts the mixing proportion of the solvent by controlling the opening and closing time, and the medium valve (106) can be switched into three states, namely pipeline closing, gas pipeline communication and liquid pipeline communication.
3. The multi-channel pressure solvent extractor system flow path of claim 1, wherein: and a manual plug valve (302) is arranged on the upper sealing seat (301) and can be used for manually relieving pressure.
4. The multi-channel pressure solvent extractor system flow path of claim 1, wherein: the end of heating collection pipeline (402) sets up collects the needle, the end of exhaust pipeline (404) sets up the waste gas needle, place a plurality of collecting bottle in collecting subassembly (403), collecting subassembly (403) rises to remove the confession the collection needle reaches the waste gas needle pierces through the top seal pad of collecting bottle.
5. An application method of a flow path of a multi-channel pressure solvent extraction instrument system is characterized by comprising the following steps:
step 1, placing a test flow, wherein a sample is loaded into an extraction tank (304) and placed on a heating body (303), a sealing mechanism (306) controls an upper sealing seat (301) to move downwards, the upper sealing seat (301) moves downwards together by pressing the extraction tank (304) on the heating body (303), the bottom end of the extraction tank (304) moves to a lower sealing seat (305), at the moment, the upper sealing seat (301) and the lower sealing seat (305) are respectively in contact sealing with the top end and the bottom end of the extraction tank (304), a collection mechanism (406) drives a collection assembly (403) and a collection bottle to move upwards together, and a top sealing gasket of the collection bottle is pierced by a collection needle and an exhaust gas needle respectively;
step 2, closing a lower sealing valve (401), opening an upper sealing valve (203), adjusting a medium valve (106) from a closed pipeline state to a gas pipeline open state, and communicating with a gas source (107), opening the gas source (107) and briefly inflating the extraction tank (304), closing the upper sealing valve (203), comparing the recorded values of a total pressure sensor (108) and each channel pressure sensor (204), determining that the placement position of the extraction tank (304) is correct, and otherwise, determining that the placement position of the extraction tank (304) is incorrect, and readjusting the placement position of the extraction tank (304) until the placement position is correct;
step 3, a temperature rise process, wherein the upper sealing valve (203) is opened again, the heating body (303) starts to heat, the medium valve (106) is adjusted to a liquid pipeline communication state from a gas pipeline opening state, the infusion pump (104) is opened, the proportional valve (102) controls the flow rate of each solvent by adjusting the opening time, the purpose of adjusting the solvent ratio is achieved, each solvent flows into the mixer (103) to be mixed to form a mixed solvent, and the mixed solvent is conveyed to the extraction tank (304) through the infusion pump (104);
step 4, a boosting process, wherein a boosting stage in the extraction tank (304) is divided into two stages, namely a pre-full pressure stage and a method pressure stage, the pre-full pressure stage is to preheat the extraction tank (304) through the heating body (303) so that a normal-temperature mixed solvent injected into the extraction tank (304) can be preheated, a certain pressure can be released in the preheating process, the preheating can enable the pressure of a static extraction stage to be more stable, if the pre-full pressure stage is not carried out and the method pressure stage is directly carried out, the method pressure setting is directly carried out, the pressure in the extraction tank (304) is enabled to reach the method set pressure in advance, the boosting process adopts a PID program to boost the pressure, and the boosting efficiency and accuracy of the stage are ensured;
if the pressure does not rise within a certain time in the boosting process, the composite emptying valve (105) is opened to empty the gas or bubbles in the liquid pipeline, the composite emptying valve (105) is closed, and the infusion pump (104) continues to inject the mixed solution into the extraction tank (304);
step 5, an extraction process, wherein the temperature of the extraction tank (304) is raised to a method temperature by the heating body (303), and when the pressure is raised to a method pressure, the infusion pump (104), the medium valve (106) and the upper sealing valve (203) are closed, the mixed solvent in the extraction tank (304) is kept at the method temperature and the method pressure, and a static extraction stage is started;
the static extraction stage is divided into three modes of standard extraction, constant pressure extraction and flow extraction;
in the standard extraction mode, the pressure rise and the pressure drop in the extraction tank (304) are not processed, the extraction efficiency is generally dependent on the temperature rather than the pressure, and the change of the pressure has little influence on the extraction result;
in a constant pressure extraction mode, the pressure of each channel is monitored through the whole process of each channel pressure sensor (204), and pressure compensation or pressure relief is carried out after the pressure abnormality of the extraction tank (304) of the corresponding channel exceeds a certain range;
the pressure supplementing process is that the upper sealing valve (203) of the corresponding channel is opened, the infusion pump (104) is opened, mixed solvent is injected into the extraction tank (304) needing pressure supplementing, and after the pressure in the extraction tank (304) with abnormal pressure is recovered to the method pressure, the infusion pump (104) and the upper sealing valve (203) of the corresponding channel are closed until the static extraction process is finished;
in the pressure relief process, the lower sealing valve (401) of the corresponding channel is slowly opened, so that the extracting solution in the extraction tank (304) needing pressure relief flows into the corresponding collection bottle in the collection assembly (403) through the lower sealing valve (401), meanwhile, the pressure in the channel is judged in real time through the channel pressure sensor (204), and after the pressure is relieved to the method pressure, the lower sealing valve (401) is quickly closed until the static extraction process is finished;
in a flow extraction mode, after entering a static extraction process, opening each lower sealing valve (401) by a certain margin, monitoring the channel pressure sensor (204) to know that the pressure in each extraction tank (304) is reduced by a small margin, at this time, stopping the opening margin of the lower sealing valve (401), and keeping the current state, meanwhile, as in the above-mentioned method in the pressure compensation process, opening the infusion pump (104), continuously injecting the mixed solvent into the extraction tank (304) needing pressure compensation, and simultaneously continuously flowing the extracting solution in the extraction tank (304) into the corresponding collection bottle in the collection assembly (403), so that the pressure in the extraction tank (304) can be kept within a method pressure range until the static extraction process is finished;
step 6, a collecting process, wherein the upper sealing valve (203) and the lower sealing valve (401) are opened, extracting solution flows into the collecting bottle by using the pressure in the extraction tank (304), the collecting process is finished after the pressure is sensed to be reduced to a set value by the channel pressure sensor (204), and in the collecting process, the heating and collecting pipeline (402) is always in an open state, so that the extracting solution can be kept in a set temperature range in the heating and collecting pipeline (402), and the extracting solution containing grease or other extracting solutions which are easy to condense due to the reduction of temperature and pressure is prevented from blocking the pipeline;
and 7, a flushing process, wherein the upper sealing valve (203), the lower sealing valve (401) and the infusion pump (104) are opened, the extraction tank (304) and the pipeline are cleaned through the infusion pump (104), then the flushing process is carried out, the purging process is carried out, the gas source (107) is used for carrying out gas purging on the extraction tank (304) and the pipeline, waste liquid and waste gas generated by flushing and purging enter the collecting bottle, and the waste gas is discharged outwards through the waste discharge pipeline (404) and the waste discharge concentration block (405).
CN202210716018.6A 2022-06-22 2022-06-22 Flow path of multi-channel pressure solvent extraction instrument system and application method Pending CN115155099A (en)

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