Automatic extraction separation system and automatic extraction separation method

Abstract

The invention provides an automatic extraction separation system and an automatic extraction separation method, and relates to the technical field of solid-phase extraction. The automatic extraction and separation system comprises: a sample introduction device, which comprises a telescopic batcher and a telescopic constant volume device, the batcher is used for extracting a sample by weight, and the constant volume device is used for extracting a solvent by volume; the extraction device comprises a rack, and at least one sample disc assembly, an extraction disc assembly, a collection disc assembly and an image collector which are mounted on the rack; the sample introduction device and the extraction device are both in circuit connection with the control panel, and the control panel is used for controlling the sample introduction device and the extraction device. According to the automatic extraction and separation system, full-automatic operation can be achieved, and the extraction efficiency and the extraction precision are improved through accurate control over constant volume and quantification.

Description

Technical Field

[0001] This application relates to the field of petrochemical technology, and in particular to an automatic extraction and separation system and an automatic extraction and separation method. Background Technology

[0002] With the continuous development and upgrading of analytical technology, testing technology is changing rapidly. Analytical instruments are gradually developing towards higher levels of automation and intelligence. People not only require accurate and reliable sample separation and extraction, but also demand more timely, efficient and automated processing and analysis.

[0003] Solid-phase extraction (SPE) is a commonly used method in laboratory analysis, which can improve the recovery rate of analytes compared to traditional liquid-phase extraction. The extractant in SPE is a solid. Current SPE technologies rely on full automation to achieve stirring and separation during the extraction process. However, sample collection, and the collection of the upper and lower layers of the extracted liquid all require manual control and settings, resulting in a very low level of automation and susceptibility to human error. Furthermore, during the extraction process, laboratory personnel are exposed to harmful volatile solvents, posing a threat to their health.

[0004] Therefore, how to rationally design an extraction instrument and accurately extract liquid extracts through constant volume and quantitative analysis has become a pressing problem that needs to be solved. Summary of the Invention

[0005] In view of the above problems, embodiments of this application provide an automated extraction and separation system and an automated extraction and separation method. The above-mentioned automated extraction and separation system can achieve fully automated operation, and improve extraction efficiency and accuracy through precise control of volume and quantity.

[0006] To achieve the above objectives, the embodiments of this application provide the following technical solutions:

[0007] On one hand, embodiments of this application provide an automated extraction and separation system, comprising:

[0008] The sample injection device includes a retractable metering device and a retractable container, the metering device being used to extract the sample by weight and the container being used to extract the solvent by volume.

[0009] The liquid addition device includes multiple solvent bottles, which are fixedly mounted on the frame below the sample injection device and are used to add solvent to the extraction disk assembly;

[0010] An extraction apparatus includes a frame and at least one sample tray assembly, an extraction tray assembly, a collection tray assembly, and an image acquisition device mounted on the frame; the sample tray assembly is used to dissolve the sample, the extraction tray assembly is used to separate the sample into different products, the collection tray assembly is used to collect the separated products, and the image acquisition device is used to acquire image information from the extraction tray assembly.

[0011] The control panel, sample injection device, and extraction device are all electrically connected to the control panel, which is used to control the sample injection device and extraction device.

[0012] The collection tray assembly includes a collection tray and multiple collection bottles, which are placed on the collection tray;

[0013] The collecting plate assembly and the extraction plate assembly are connected by a multi-way valve, which transports the different products separated by the extraction plate assembly to different collecting bottles.

[0014] The extraction disc assembly separates up to three products, the collection disc assembly is provided with at least three collection bottles, and the multi-way valve is a four-way valve that delivers the three products to the three collection bottles respectively.

[0015] The image acquisition unit is mounted on the rack via a drive unit, which drives the image acquisition unit to move up and down along the height of the extraction disc assembly.

[0016] The extraction disc assembly includes an extraction disc and multiple extraction columns, with the extraction columns placed on the extraction disc.

[0017] An extraction port is provided at the bottom of the extraction column, and a control valve is connected to the extraction port. The control valve is connected to the control panel circuit.

[0018] The extraction column consists of a column body and a column head, with the column head being detachably connected to the bottom of the column body. A control valve is connected to the column head.

[0019] The sample tray assembly includes a sample tray, a heating plate, and multiple sample tubes. The sample tubes are placed on the sample tray, and the heating plate is located at the bottom of the sample tray.

[0020] The extraction device includes a first sample tray assembly and a second sample tray assembly. The first sample tray assembly is used to dissolve the sample, and the second sample tray assembly is used to store a preset weight of sample and continue to dissolve the sample.

[0021] The first sample tray assembly and the second sample tray assembly are arranged sequentially on the same side of the extraction tray assembly.

[0022] On the other hand, embodiments of this application provide an automated extraction and separation method, including:

[0023] The sample is extracted into the sample tray assembly of the extraction device by controlling the metering device through the control panel. The sample tray assembly is then used to heat the sample to melt it.

[0024] The metering device and the container are controlled by the control panel to extract the preset weight of sample and solvent. After the sample is fully dissolved, the sample is injected into the extraction plate assembly of the extraction device.

[0025] Different solvents are sequentially added to the extraction plate assembly through a fixed container to separate the stationary phase in the sample into different products, which are then collected in the collection plate assembly of the extraction device. Meanwhile, the image acquisition device in the extraction device acquires image information of the stationary phase to determine the separated products.

[0026] The extraction disk assembly includes an extraction disk and multiple extraction columns. After the sample is injected into the extraction columns, it includes:

[0027] The first solvent and the second solvent are added sequentially to the extraction column using a fixed container to separate the first product from the stationary phase, and the first product is collected in the first collection bottle of the collection tray assembly;

[0028] The second solvent and the third solvent are added to the stationary phase in sequence using a fixed container. When the image acquisition device detects that the colloidal ring in the stationary phase has moved to the target position, the second product in the stationary phase is separated and collected in the second collection bottle in the collection tray assembly.

[0029] A third solvent is added to the stationary phase using a fixed container to separate the third product from the stationary phase, and the third product is collected in the third collection container in the collection tray assembly.

[0030] The extraction port at the bottom of the extraction column is connected to a control valve, and a four-way valve is connected between the collection tray assembly and the control valve.

[0031] During the separation of the first product, the control valve is opened, and the four-way valve connects the extraction column and the first collection bottle;

[0032] During the separation of the second product, the control valve is opened, and the four-way valve is switched to connect the extraction column and the second collection bottle;

[0033] When the image acquisition device detects that the gel ring has moved to the target position, the control valve closes first, and the four-way valve switches to connect the extraction column and the third collection bottle, and then the control valve opens again.

[0034] The image acquisition device captures the movement of the gelatinous ring to the target location, including:

[0035] The image acquisition device captured the colloidal ring moving downwards to the bottom of the extraction column.

[0036] The extraction apparatus includes a first sample tray assembly and a second sample tray assembly. Before injecting the sample into the extraction tray assembly, it includes:

[0037] The sample is heated using the first sample tray assembly to melt it;

[0038] A sample of a predetermined weight is extracted using a metering device and injected into the second sample pan assembly. A first solvent is then added to the second sample pan assembly using a fixed container to ensure that the sample is fully dissolved.

[0039] This application provides an automated extraction and separation system and method. The automated extraction and separation system includes a sample injection device, an extraction device, a liquid addition device, and a control panel. Specifically, the sample injection device includes a retractable metering device and a retractable container. The metering device is used for quantitative extraction of the sample, and the container is used for volumetric extraction of the solvent. The extraction device includes a frame and at least one sample tray assembly, an extraction tray assembly, a collection tray assembly, and an image acquisition device mounted on the frame. The frame connects and fixes the sample tray assembly, extraction tray assembly, collection tray assembly, and image acquisition device. Two sample tray assemblies and the extraction tray assembly are located in the middle of the frame, and the collection tray assembly is located at the lower part of the frame. The sample tray assembly is used to heat and dissolve the sample, the extraction tray assembly is used to separate the sample into different products, and the collection tray assembly is used to collect the separated products. The image acquisition device is connected to the control panel and the extraction tray assembly to acquire image information from the extraction tray assembly. The control panel is electrically connected to the sample injection device and the extraction device, and can control the container, metering device, sample tray assembly, extraction tray assembly, collection tray assembly, and image acquisition device respectively. In this way, the control panel can precisely control the fully automated extraction and separation process, realizing the entire process from sampling to extraction, and from extraction to separation. Simultaneously, a real-time image acquisition device can be used for monitoring, avoiding the influence of human judgment regarding the color and position of the colloidal rings, thus improving the accuracy of extraction.

[0040] In addition to the technical problems solved by the embodiments of this application, the technical features constituting the technical solutions, and the beneficial effects brought about by the technical features of these technical solutions described above, other technical problems that can be solved by the automatic extraction and separation system and automatic extraction and separation method provided by the embodiments of this application, other technical features included in the technical solutions, and the beneficial effects brought about by these technical features will be further explained in detail in the specific implementation. Attached Figure Description

[0041] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0042] Figure 1 A schematic diagram of the front view of the automated extraction and separation system provided in the embodiments of this application;

[0043] Figure 2 for Figure 1 A schematic diagram of the sample introduction device in the diagram;

[0044] Figure 3 This is a top view schematic diagram of the automated extraction and separation system provided in the embodiments of this application;

[0045] Figure 4 This is a schematic diagram showing the positional relationship between the image acquisition device and the extraction column provided in an embodiment of this application;

[0046] Figure 5 A schematic diagram illustrating the connection relationship between the multi-way valve and the collection bottle provided in an embodiment of this application;

[0047] Figure 6 This is a schematic diagram of the extraction column provided in an embodiment of this application;

[0048] Figure 7 A flowchart illustrating the steps of the automated extraction and separation method provided in this application embodiment.

[0049] Explanation of reference numerals in the attached figures:

[0050] 10-Automatic extraction and separation system;

[0051] 100 - Sample injection device; 200 - Extraction device; 300 - Liquid addition device; 400 - Control panel;

[0052] 110 - Quantitative analyzer; 120 - Container; 210 - Frame; 220 - Sample tray assembly; 230 - Extraction tray assembly; 240 - Collection tray assembly; 250 - Image acquisition device; 310 - Solvent bottle;

[0053] 111-First telescopic rod; 112-Quantitative needle; 121-Second telescopic rod; 122-Volume-adjusting needle; 211-Driver; 220a-First sample tray assembly; 220b-Second sample tray assembly; 221-Sample tray; 222-Heating tray; 223-Sample tube; 231-Extraction tray; 232-Extraction column; 241-Collection tray; 242-Collection bottle; 243-Multi-port valve;

[0054] 2200 - Disc; 2321 - Column; 2322 - Column head; 2323 - Control valve; 2421 - First collection bottle; 2422 - Second collection bottle; 2423 - Third collection bottle;

[0055] 2321a - Sieve plate; 2321b - Gasket. Detailed Implementation

[0056] As described in the background section, in related technologies, the sampling process and the collection of the upper and lower layers of the extracted liquid in automated extraction and separation systems typically require manual control and setting. Specifically, operating the sample container or collecting the separated products requires human assistance or intervention to ensure the coordination of the various devices within the extraction and separation system.

[0057] However, the aforementioned extraction and separation methods have extremely low automation and are easily affected by human error. During the extraction process, personnel come into contact with harmful volatile solvents, which can adversely affect their health and even threaten their lives. Therefore, achieving a fully automated extraction and separation process, rationally designing the extraction instrument, and accurately extracting the liquid extract through constant volume and quantitative analysis have become pressing problems that need to be solved.

[0058] In view of this, embodiments of this application provide an automated extraction and separation system and an automated extraction and separation method. The automated extraction and separation system includes a sample introduction device, an extraction device, and a control panel. Specifically, the sample introduction device includes a retractable metering device and a retractable container. The metering device is used for quantitative extraction of the sample, and the container is used for volumetric extraction of the solvent. The extraction device includes a frame and at least one sample tray assembly, an extraction tray assembly, a collection tray assembly, and an image acquisition device mounted on the frame. The frame connects and fixes the sample tray assembly, extraction tray assembly, collection tray assembly, and image acquisition device. The sample tray assembly is used to heat the sample, the extraction tray assembly is used to separate the sample into different products, and the collection tray assembly is used to collect the separated products. The image acquisition device is connected to the control panel and the extraction tray assembly to acquire image information from the extraction tray assembly. The control panel is electrically connected to the sample introduction device and the extraction device, and can control the container, metering device, sample tray assembly, extraction tray assembly, collection tray assembly, and image acquisition device respectively. Thus, the control panel can precisely control the fully automated extraction and separation process, realizing the entire process from sampling to extraction, and from extraction to separation. Simultaneously, real-time monitoring using an image acquisition device avoids the influence of human judgment regarding the color and position of the colloidal rings, improving the accuracy of extraction. In this way, the control panel can precisely control the fully automated extraction and separation process, realizing the entire process from sampling to extraction, and from extraction to separation. Furthermore, real-time monitoring using an image acquisition device avoids the influence of human judgment regarding the color and position of the colloidal rings, improving the accuracy of extraction.

[0059] To make the above-mentioned objectives, features, and advantages of the embodiments of this application more apparent and understandable, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0060] Figure 1 This is a schematic diagram of the front view of the automated extraction and separation system provided in an embodiment of this application. (Refer to...) Figure 1As shown, the automated extraction and separation system 10 is applicable to solid-phase extraction. By adjusting parameters such as the type and concentration of the solvent, heating temperature, and droplet flow rate, the extraction process can be precisely controlled to obtain high-purity target components. For example, the automated extraction and separation system 10 is applied to the composition analysis of heavy distillate oils.

[0061] Specifically, the automated extraction and separation system 10 includes a sample injection device 100, an extraction device 200, a liquid addition device 300, and a control panel 400. The sample is supplied to the extraction device 200 as needed using the sample injection device 100 and the liquid addition device 300. The extraction device 200 extracts and separates the sample for component analysis. The control panel 400 is electrically connected to the sample injection device 100, the extraction device 200, and the liquid addition device 300. The control panel 400 controls the operation of the sample injection device 100, the extraction device 200, and the liquid addition device 300 to achieve fully automated operation of the automated extraction and separation system. The liquid addition device 300 includes multiple solvent bottles 310, which are fixedly installed below the sample injection device 100 for adding solvent during the extraction process.

[0062] Figure 2 for Figure 1 A schematic diagram of the sample introduction device 100. (Refer to...) Figure 2 As shown, the sample injection device 100 includes a retractable metering device 110 and a retractable container 120. The metering device 110 is used to extract the sample by weight, and the container 120 is used to extract the solvent in the solvent bottle 310 by volume.

[0063] Specifically, the metering device 110 includes a first telescopic rod 111 and a metering needle 112. One end of the first telescopic rod 111 is connected to the sample injection device 100, and the metering needle 112 is located at the other end of the first telescopic rod 111. The metering needle 112 has a weighing function and can accurately extract the sample by mass. The volumetric container 120 includes a second telescopic rod 121 and a volumetric needle 122. One end of the second telescopic rod 121 is connected to the sample injection device 100, and the volumetric needle 122 is located at the other end of the second telescopic rod 121. The volumetric needle 122 can add solvent to the sample and the extraction column 232 according to a set volume. The volumetric needle 122 is located at the lower end of the second telescopic rod 121.

[0064] Using the metering device 110 and the volumetric calibrator 120 separately can effectively prevent sample contamination, and the metering needle 112 and the volumetric calibrator 122 can be automatically discarded and replaced to avoid cross-contamination between samples. Volumetric and quantitative analysis can further standardize the operating procedure.

[0065] The extraction apparatus 200 includes a frame 210, at least one sample tray assembly 220, an extraction tray assembly 230, and a collection tray assembly 240. The frame 210 serves as the basic support structure, and the sample introduction device 100, sample tray assembly 220, extraction tray assembly 230, and collection tray assembly 240 are all mounted and fixed to the frame. Exemplarily, the sample introduction device 100 is located on the left side of the extraction apparatus 200, wherein the sample tray assembly 220 and extraction tray assembly 230 can be mounted and fixed to the middle of the frame 210, and the collection tray assembly 240 can be mounted and fixed to the lower part of the frame 210. Exemplarily, the sample tray assembly 220 is located to one side of the extraction tray assembly 230, and the collection tray assembly 240 is located below the extraction tray assembly 230. The outer edges of the extraction tray assembly 230 and the extraction liquid collection tray assembly 240 overlap, and the support hole of the extraction tray assembly 230 is located above the support hole of the extraction liquid collection tray assembly 240 to facilitate experimental operation.

[0066] Specifically, the sample tray assembly 220 includes a sample tray 221, a heating plate 222, and multiple sample tubes 223. The sample tubes 223 are placed in the sample tray 221, and the heating plate 222 is located at the bottom of the sample tray 221. The heating plate 222 has a built-in thermostatic heater. In this embodiment, heavy oil is used as the sample. Because heavy oil has high viscosity, it is usually a viscous liquid or solid at room temperature with poor fluidity. It can only flow after being heated by the heating plate 222. The temperature of the heating plate 222 is controlled between 40 and 80°C.

[0067] In this embodiment, there are two sample tray assemblies 220: a first sample tray assembly 220a and a second sample tray assembly 220b. The first sample tray assembly 220a is used to heat and melt the sample, while the second sample tray assembly 220b is used to store a preset weight of sample and continue dissolving the sample. Of course, the first sample tray assembly 220a and the second sample tray assembly 220b can be combined into one for both sample dissolution and storage.

[0068] The extraction disk assembly 230 is used to separate a sample into different products. The extraction disk assembly 230 includes an extraction disk 231 and multiple extraction columns 232. The sample solution to be separated is loaded onto the extraction columns 232, where the target compound in the sample undergoes specific interactions with the stationary phase (such as adsorption, ion exchange, etc.), thus being retained on the stationary phase. The target compound is then eluted by a mobile phase (such as a solvent). Because the extraction column 232 has an extraction port at its bottom, separation of the upper and lower liquid layers can be achieved.

[0069] The collecting tray assembly 240 is used to collect the fractions. During elution, the target compound flows out with the solvent. The outflowing solution is collected in stages based on the liquid level recognition by the image acquisition device 250. The collecting tray assembly 240 includes a collecting tray 241 and multiple collecting bottles 242. The collecting bottles 242 are placed in the collecting tray 241 to collect the separated products in the collecting bottles 242.

[0070] Figure 3 This is a top view schematic diagram of the automated extraction and separation system provided in an embodiment of this application. (In conjunction with...) Figure 1 and Figure 3 As shown, the sample plate 221, extraction plate 231 and collection plate 241 of the extraction device 200 are all circular plates with multiple holes 2200 arranged circumferentially. In this embodiment, there are a total of 8 holes 2200.

[0071] Figure 4 This is a schematic diagram illustrating the positional relationship between the image acquisition device and the extraction column provided in an embodiment of this application. (Refer to...) Figure 4 As shown, the extraction device 200 also includes an image acquisition unit 250, which is mounted on the frame 210 via a drive unit 211. The drive unit 211 drives the image acquisition unit 250 to move, thereby enabling the image acquisition unit 250 to move up and down along the height direction of the extraction column 232. Exemplarily, the drive unit 211 can be a slide rod, a pneumatic rod, a hydraulic rod, a lead screw, a telescopic rod, etc., and this embodiment does not impose specific limitations on it.

[0072] At least one extraction column 232 is placed in the extraction tray 231, and in this embodiment, up to eight extraction columns 232 are placed there, with the extraction columns 232 circumferentially spaced within the tray holes. The extraction tray 231 is fixedly connected by a frame 210. An image acquisition device 250 is located directly in front of the extraction column 232 and parallel to it. The image acquisition device 250 acquires images of the extraction column 232 in real time, records the downward movement of the colloidal ring, and moves downward along with it in the height direction of the extraction column 232 via a drive component 211 until the image acquisition device 250 is level with the lower end of the extraction column 232. In this embodiment, the horizontal distance between the image acquisition device 250 and the extraction column 232 is set to 1-3 cm. By acquiring images of the color change at the orthographic projection position of the fixed phase in the extraction column 232, the separated product can be accurately determined. The downward movement of the liquid separation interface is fed back to the control system for subsequent extraction operations.

[0073] Figure 5 This is a schematic diagram illustrating the connection relationship between the multi-way valve and the collection bottle provided in an embodiment of this application. (In conjunction with...) Figure 3 and Figure 5 , Figure 3The image shows that the extraction plate 231 and the collection plate 241 are connected by a multi-way valve 243. The multi-way valve 243 connects different collection containers 242 on the collection plate 241 to the extraction column 232, allowing different extracted products to be collected into different collection containers 242. In this embodiment, taking three products as an example, the multi-way valve 243 can be a four-way valve. The inlet of the four-way valve is connected to the extraction column 232, and the three outlets of the four-way valve are respectively connected to the three collection containers 242. The multi-way valve 243 is mainly used to regulate and switch the flow direction of the liquid during the chemical extraction process. Furthermore, the multi-way valve 243 is connected to the control panel 400, which controls the liquid flow, enabling remote control and monitoring, improving the automation level of the extraction process, reducing manual intervention, and significantly increasing production efficiency. The aforementioned four-way valve has four interchange ports: a, b, c, and d. The four-way valve interchange port d is connected to the outlet of the extraction column 232. The other three transfer outlets of the four-way valve are connected to the collection tray 241. After the sample is extracted, the extract is collected into the first collection bottle 2421, the second collection bottle 2422, and the third collection bottle 2423, respectively.

[0074] Figure 6 This is a schematic diagram of the extraction column 232 provided in an embodiment of this application. (Refer to...) Figure 6 As shown, the extraction column 232 includes a column body 2321 and a column head 2322. The column head is connected to the bottom end of the main body, and the column body 2321 and the column head 2322 are separable. The column body 2321 serves as the basic structure of the extraction column 232, and contains packing material. The sample extraction process is mainly carried out within the column body 2321. An extraction port is provided at the bottom end of the column head 2322. The extracted and separated product is discharged from the extraction port at the bottom end of the column head and collected in the collection tray assembly 240.

[0075] A sieve plate 2321a and a gasket 2321b are stacked at the bottom of the column 2321, with the sieve plate 2321a stacked on top of the gasket 2321b. Specifically, taking a circular cross-sectional shape of the column 2321 as an example, the outline shape of the sieve plate 2321a can also be circular to adapt to the cross-sectional shape of the column 2321. The sieve plate 2321a is used to support and fix the solid packing material inside the extraction column 232, preventing the packing material from moving or leaking during the process. Furthermore, the sieve plate 2321a utilizes its uniformly distributed sieve holes to ensure sufficient contact between the fluid and the solid packing material, improving extraction efficiency. The gasket 2321b is located at the joint of the column 2321. In this embodiment, the gasket 2321b is located below the sieve plate 2321a, between the column head 2322 and the sieve plate 2321a. The gasket 2321b is mainly used to provide a seal between the components of the extraction column 232 to prevent liquid leakage.

[0076] Continue to refer to Figure 6An extraction port at the bottom of the extraction column 232 is connected to a control valve 2323, which can be a solenoid valve. The control valve 2323 is electrically connected to the control panel 400. The control valve 2323 can precisely control the fluid flow at the bottom of the extraction column 232, ensuring that the sample and solvent pass through the extraction column 232 at appropriate times and rates. Furthermore, the control valve 2323 can be quickly opened or closed as needed, thereby achieving precise separation of different components, automated operation, and improving the accuracy of extraction.

[0077] Figure 7 A flowchart illustrating the steps of the automated extraction and separation method provided in this application embodiment. (Refer to...) Figure 7 As shown in the embodiments of this application, the automatic extraction and separation method (hereinafter referred to as the extraction and separation method) includes the following steps:

[0078] S100: The sample is extracted into the sample tray assembly of the extraction device by controlling the metering device and the container through the control panel, and the sample is heated by the sample tray assembly to melt the sample.

[0079] The oil sample is first placed into the sample tube 223 in the first sample tray assembly 220a. The control panel 400 of the automatic extraction and separation system 10 is then activated, and the sample is heated using the heating plate 222 in the sample tray assembly 220. For example, taking heavy distillate oil as an example, the heating plate temperature can be set to 60°C. The control panel 400 can control the temperature of the heating plate 222.

[0080] The quantitative needle 112 in the injection device 100 will draw a preset mass of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-fixing needle 122 will add a preset volume of the first solvent into the sample tube 223 of 220b. After it is fully dissolved, the volume-fixing injection needle will draw another 1-5 mL of the first solvent and add it into the solid phase extraction column 232. Then, the sample dissolved in the sample tube 223 will be drawn into the rinsed extraction column 232 by the volume-fixing needle 122.

[0081] The control panel 400 can sample a preset weight using the quantitative needle 112 and control the quantitative device 110 and the fixed container 120 to transfer the sample between the sample tray assembly 220 and the extraction tray assembly 231. The control panel 400 enables precise quantitative operation and improves experimental efficiency.

[0082] S200: Different solvents are added sequentially to the extraction plate assembly through a fixed container to separate the stationary phase in the sample into different products, and the different products are collected in the collection plate assembly of the extraction device; wherein, the image information of the stationary phase is acquired by the image acquisition device in the extraction device to determine the separated products.

[0083] The stationary phase is then washed sequentially with quantitative amounts of the first and second solvents to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first extraction collection bottle 2421. The stationary phase is then further eluted with the second solvent until it is completely absorbed. Finally, the stationary phase is washed with a third solvent. The image acquisition unit 250 gradually slides downwards along the drive unit 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. As the colloidal rings in the stationary phase gradually descend until they reach the bottom of the extraction column 232, aromatic hydrocarbons are eluted and collected in the second extraction collection bottle 2422. The stationary phase is then further washed with the third solvent, and the eluted colloids are collected in the third extraction collection bottle 2423.

[0084] The four-way valve first switches to the first collection bottle 2421 of the extract, eluting saturated hydrocarbons into it with a preset volume of solvent. Then, the four-way valve switches to the second collection bottle 2422 of the extract, adding preset second and third solvents. When the image acquisition device 250 detects a colloidal ring in the extraction column 232 and it moves to the bottom of the column, the solenoid valve at the bottom of the column 232 is closed. At this point, the four-way valve switches to the third collection bottle 2423 of the extract, and the control valve 2323 at the bottom of the column 232 is opened. The solid-phase extraction column is then rinsed with a preset volume of third solvent, flushing the colloidal material into the third collection bottle 2423 of the extract.

[0085] For example, the first solvent is a low-carbon n-alkanes, the second solvent is a low-carbon haloalkanes, and the third solvent is a mixed solution of low-carbon haloalkanes and alcohols in a volume ratio of 1:1 to 1:5.

[0086] In this embodiment, the first product, the second product, and the third product are saturated hydrocarbon, aromatic hydrocarbon, and gum, respectively.

[0087] Taking heavy oil as an example, the following is a detailed operation flow of the automatic extraction and separation method provided in the embodiments of this application. This operation flow is applicable to the above-mentioned automatic extraction and separation device.

[0088] Combination Figure 1 and Figure 3 As shown, on the control panel 400, the heating temperature of the heating plate 222 is set to 50-60℃, and heavy oil is placed into the sample tube 223 in the first sample plate assembly 220a. When the sample melts into a liquid, the quantitative needle 112 in the injection device 100 draws 0.1-0.2g of sample from the sample tube 223 of the first sample plate assembly 220a and places it into the sample tube 223 of the second sample plate assembly 220b. Then, the volumetric needle 122 adds 1-2mL of the first solvent to the sample tube 223 of the second sample plate assembly 220b to fully dissolve the sample.

[0089] After the sample is fully dissolved, the extraction plate assembly 230 is activated, and the volume-dilution needle 122 draws another 1-2 mL of the first solvent and adds it to the solid-phase extraction column 232. Then, the heavy oil dissolved in the sample tube 223 of the second sample plate assembly 220b is drawn into the rinsed extraction column 232 using the volume-dilution needle 122. The stationary phase is then washed with 3-5 mL of the first solvent and 1-2 mL of the second solvent in sequence to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. The stationary phase is then eluted with 3-5 mL of the second solvent. When the second solvent has completely entered the stationary phase, the solid-phase extraction column 232 is washed with 3-5 mL of the third solvent. The image acquisition device 250 slides down along the drive component 211 to monitor and identify the color and position of the colloidal ring in the extraction column 232. When the colloidal rings in the stationary phase gradually descend until they move to the bottom of the solid-phase extraction column 232, the eluted material is aromatic hydrocarbon, which is collected in the second collection bottle 2422. The solid-phase extraction column 232 is then rinsed with 3-5 mL of the third solvent, and the eluted colloids are collected in the third collection bottle 2423.

[0090] During this process, the multi-way valve 243 first switches to the first collection bottle 2421, eluting saturated hydrocarbons into the first collection bottle 2421 according to the preset volumes of the first and second solvents. Then, the multi-way valve 243 switches to the second collection bottle 2422, and continues to add the preset second and third solvents. When the image acquisition device 250 detects the appearance of a colloidal ring in the solid-phase extraction column 232 and moves to the bottom of the extraction column 232, it closes the solenoid valve at the bottom of the extraction column 232. At this time, the multi-way valve 243 switches to the third collection bottle 2423, and then the solenoid valve at the bottom of the extraction column 232 opens, and the solid-phase extraction column 232 is rinsed with the preset volume of the third solvent, flushing the colloidal substance into the third collection bottle 2423.

[0091] The first solvent is a low-carbon n-alkanes (preferably such as n-butane, n-pentane, n-hexane, etc.), the second solvent is a low-carbon haloalkanes (preferably such as fluoroalkanes, monochloromethane, dichloromethane, etc.), and the third solvent is a mixed solution of low-carbon haloalkanes and alcohols (preferably such as a mixture of dichloromethane and ethanol, a mixture of dichloromethane and methanol, etc.), with a preferred volume ratio of 1:1 to 1:3. Specific implementation examples:

[0093] Example 1: Pour heavy oil sample No. 1 into sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of heating plate 222 to 60℃ on the control panel 400, draw in 0.1g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-hexane with the volume-depleting needle 122: 1mL, 1mL, 4mL, 1mL, 5 ... When the oil melts into a liquid, the automatic extraction is started. The quantitative needle 112 in the sample injection device 100 draws 0.1g of sample from the sample tube 223 of the first sample tray assembly 220a and places it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 adds 1mL of the first solvent, n-hexane, to the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 draws another 1mL of n-hexane and adds it to the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b is drawn into the rinsed extraction column 232 by the volume-dilution needle 122. The stationary phase is rinsed with 4mL of n-hexane and 1mL of dichloromethane in sequence. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. In the process, the stationary phase is eluted with 5 mL of dichloromethane. The multi-way valve 243 is switched to outlet b. When the dichloromethane has completely entered the stationary phase, the extraction column 232 is rinsed with 5 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The image acquisition device 250 gradually slides down along the drive component 211 to monitor and identify the color and position of the colloidal ring in the extraction column 232. When the image acquisition device 250 captures the colloidal ring in the stationary phase gradually descending until the colloidal ring moves to the bottom of the solid phase extraction column 232, the control valve 2323 at the bottom of the extraction column 232 is closed. At this time, the eluted material is aromatic hydrocarbon, which is collected in the second collection bottle 2422. Then, the multi-way valve 243 is switched to outlet c, the control valve 2323 is opened, and the solid phase extraction column 232 is rinsed with 5 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The eluted colloidal material is collected in the third collection bottle 2423.

[0094] The solvent in the three extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the three extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbons (WA), aromatic hydrocarbons (WB), and gums (WC) were recorded.

[0095] Finally, the weights were measured to be WA 0.0681g, WB 0.0266g, and WC 0.0017g.

[0096] The yield calculation formula is as follows:

[0097] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0098] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0099] The content of colloidal fraction in the sample, WC% = WC / (WA+WB+WC)×100%,

[0100] The calculations yielded the following for heavy oil sample No. 1: WA% was 70.64%, WB% was 27.59%, and WC% was 1.77%.

[0101] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 1 below.

[0102] Table 1. Hydrocarbon composition analysis results of heavy oil sample No. 1.

[0103]

[0104]

[0105] Example 2: Pour heavy oil sample No. 1 into sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of heating plate 222 to 60℃ on the control panel 400, draw in 0.2g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-hexane with the volume-depleting needle 122: 2mL, 2mL, 5mL, 2mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 3mL, 5mL, 1:1 mixture of dichloromethane and ethanol. When the oil melts into a liquid, the automatic extraction is started. The quantitative needle 112 in the sample injection device 100 draws 0.2g of sample from the sample tube 223 of the first sample tray assembly 220a and places it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 adds 2mL of the first solvent, n-hexane, to the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 draws another 2mL of n-hexane and adds it to the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b is drawn into the rinsed extraction column 232 by the volume-dilution needle 122. The stationary phase is rinsed with 5mL of n-hexane and 2mL of dichloromethane in sequence. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. Continue eluting the stationary phase with 3 mL of dichloromethane. Switch the multi-port valve 243 to outlet b. When the dichloromethane has completely entered the stationary phase, rinse the solid-phase extraction column 232 with 3 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The image acquisition device 250 gradually slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 captures the colloidal rings in the stationary phase gradually descending until they move to the bottom of the solid-phase extraction column 232, the control valve 2323 at the bottom of the extraction column 232 closes. At this time, the eluted material is aromatic hydrocarbons, which are collected in the second collection bottle 2422. Then, switch the multi-port valve 243 to outlet c, open the control valve 2323, and continue rinsing the solid-phase extraction column 232 with 3 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The eluted colloids are collected in the third collection bottle 2423.

[0106] The solvent in the three extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the three extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbons (WA), aromatic hydrocarbons (WB), and gums (WC) were recorded.

[0107] Finally, the weights were measured to be WA 0.0704g, WB 0.0226g, and WC 0.0022g.

[0108] The yield calculation formula is as follows:

[0109] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0110] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0111] The content of colloidal fraction in the sample, WC% = WC / (WA+WB+WC)×100%.

[0112] The calculations yielded the following for heavy oil sample No. 1: WA% 73.95%, WB% 23.75%, and WC% 2.3%.

[0113] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 2 below.

[0114] Table 2. Hydrocarbon composition analysis results of heavy oil sample No. 1.

[0115]

[0116]

[0117] Example 3: Pour heavy oil sample No. 1 into sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of heating plate 222 to 60℃ on the control panel 400, draw in 0.2g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-pentane with the volume-depleting needle 122: 2mL, 2mL, and 5mL respectively; the following volumes of the second solvent dichloromethane with the volume: 2mL and 3mL respectively; and the following volumes of the third solvent (a 1:1 mixture of dichloromethane and ethanol) with the volume: 3mL and 3mL respectively. When the oil melts into a liquid, click to start automatic extraction. The quantitative needle 112 in the sample injection device 100 will draw 0.2g of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 will add 2mL of the first solvent, n-pentane, into the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 will draw another 2mL of n-pentane and add it into the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b will be drawn into the rinsed extraction column 232 by the volume-dilution needle 122. The stationary phase will be rinsed with 5mL of n-pentane and 2mL of dichloromethane in sequence. At this time, the multi-port valve 243 will switch to outlet a to elute the adsorbed saturated hydrocarbon fraction, which will be collected in the first collection bottle 2421. Continue eluting the stationary phase with 3 mL of dichloromethane. Switch the multi-port valve 243 to outlet b. When the dichloromethane has completely entered the stationary phase, rinse the solid-phase extraction column 232 with 3 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The image acquisition device 250 gradually slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 captures the colloidal rings in the stationary phase gradually descending until they move to the bottom of the solid-phase extraction column 232, the control valve 2323 at the bottom of the extraction column 232 closes. At this time, the eluted material is aromatic hydrocarbons, which are collected in the second collection bottle 2422. Then, switch the multi-port valve 243 to outlet c, open the control valve 2323, and continue rinsing the solid-phase extraction column 232 with 3 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The eluted colloids are collected in the third collection bottle 2423.

[0118] The solvent in the three extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the three extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbons (WA), aromatic hydrocarbons (WB), and gums (WC) were recorded.

[0119] Finally, the weights were measured to be WA 0.0644g, WB 0.0296g, and WC 0.0017g.

[0120] The yield calculation formula is as follows:

[0121] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0122] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0123] The content of colloidal fraction in the sample, WC% = WC / (WA+WB+WC)×100%.

[0124] The calculations yielded the following for heavy oil sample No. 1: WA% was 67.28%, WB% was 30.88%, and WC% was 1.84%.

[0125] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 3 below.

[0126] Table 3. Hydrocarbon composition analysis results of heavy oil sample No. 1.

[0127]

[0128]

[0129] Example 4: Pour heavy oil sample No. 1 into sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of heating plate 222 to 60℃ on the control panel 400, draw in 0.1g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-pentane with the volume-depleting needle 122: 1mL, 1mL, 4mL, 1mL, 5 ... When the oil melts into a liquid, the automatic extraction is started. The quantitative needle 112 in the sample injection device 100 draws 0.1g of sample from the sample tube 223 of the first sample tray assembly 220a and places it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 adds 1mL of the first solvent, n-pentane, to the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 draws another 1mL of n-pentane and adds it to the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b is drawn into the rinsed extraction column 232 by the volume-dilution needle 122. The stationary phase is rinsed with 4mL of n-pentane and 1mL of dichloromethane in sequence. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. Continue eluting the stationary phase with 5 mL of dichloromethane. Switch the multi-port valve 243 to outlet b. When the dichloromethane has completely entered the stationary phase, rinse the solid-phase extraction column 232 with 5 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The image acquisition device 250 gradually slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 captures the colloidal rings in the stationary phase gradually descending until they move to the bottom of the solid-phase extraction column 232, the control valve 2323 at the bottom of the extraction column 232 closes. At this time, the eluted material is aromatic hydrocarbons, which are collected in the second collection bottle 2422. Then, switch the multi-port valve 243 to outlet c, open the control valve 2323, and continue rinsing the solid-phase extraction column 232 with 5 mL of a 1:1 volume ratio of dichloromethane and ethanol mixture. The eluted colloids are collected in the third collection bottle 2423.

[0130] The solvent in the three extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the three extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbons (WA), aromatic hydrocarbons (WB), and gums (WC) were recorded.

[0131] Finally, the weights were measured to be WA 0.060g, WB 0.0315g, and WC 0.0019g.

[0132] The yield calculation formula is as follows:

[0133] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0134] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0135] The content of colloidal fraction in the sample, WC% = WC / (WA+WB+WC)×100%.

[0136] The calculations yielded the following for heavy oil sample No. 1: WA% was 64.23%, WB% was 33.73%, and WC% was 2.04%.

[0137] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 4 below.

[0138] Table 4. Hydrocarbon composition analysis results of heavy oil sample No. 1.

[0139]

[0140]

[0141] Example 5: The refined oil sample No. 2 was poured into the sample tube 223 in the first sample tray assembly 220a. The automatic extraction instrument control panel 400 was started. The temperature of the heating plate 222 was set to 60°C on the control panel 400. The quantitative needle 112 drew in 0.1g of sample. The volumetric needle 122 drew in the following volumes of the first solvent n-hexane: 1mL, 1mL, and 4mL, respectively. The volume of the second solvent dichloromethane: 1mL and 5mL, respectively. The volume of the third solvent (a 1:1 mixture of dichloromethane and ethanol): 5mL and 5mL, respectively. When the oil melts into a liquid, click to start automatic extraction. The quantitative needle 112 in the injection device 100 will draw 0.1g of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 will add 1mL of the first solvent, n-hexane, into the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 will draw another 1mL of n-hexane and add it to the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b will be drawn into the rinsed extraction column 232 by the volume-dilution needle 122. This process is repeated using 4mL of the same solvent. The stationary phase is rinsed with hexane and 1 mL of dichloromethane. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. The stationary phase is then eluted with 5 mL of dichloromethane. The multi-port valve 243 is switched to outlet b. When the dichloromethane has completely entered the stationary phase, the solid phase extraction column 232 is rinsed with 5 mL of a 1:1 volume ratio mixture of dichloromethane and ethanol. The image acquisition device 250 slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 does not capture the appearance of colloidal rings in the stationary phase, the eluted fraction is aromatic hydrocarbon, which is collected in the second collection bottle 2422.

[0142] The solvent in the two extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the two extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbon WA and aromatic hydrocarbon WB were recorded.

[0143] Finally, the weights were measured: WA = 0.0797g and WB = 0.0173g.

[0144] The yield calculation formula is as follows:

[0145] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0146] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0147] Calculations showed that the refined oil sample No. 2 had a WA% of 82.16% and a WB% of 17.84%.

[0148] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 5 below.

[0149] Table 5. Hydrocarbon composition analysis results of the distillate of refined oil sample No. 2.

[0150]

[0151]

[0152] Example 6: Pour the refined oil sample No. 2 into the sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of the heating plate 222 to 60°C on the control panel 400, draw in 0.2g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-hexane with the volume-depleting needle 122: 2mL, 2mL, and 5mL respectively; the following volumes of the second solvent dichloromethane with the volume: 2mL and 3mL respectively; and the following volumes of the third solvent (a 1:1 mixture of dichloromethane and ethanol with a volume ratio of 3mL and 3mL respectively). When the oil melts into a liquid, click to start automatic extraction. The quantitative needle 112 in the sample injection device 100 will draw 0.2g of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 will add 2mL of the first solvent, n-hexane, into the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 will draw another 2mL of n-hexane and add it into the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b will be drawn into the rinsed extraction column 232 by the volume-dilution needle 122. This process is repeated using 5mL of the same solvent. The stationary phase is rinsed with hexane and 2 mL of dichloromethane. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. The stationary phase is then eluted with 5 mL of dichloromethane. The multi-port valve 243 is switched to outlet b. When the dichloromethane has completely entered the stationary phase, the solid phase extraction column 232 is rinsed with 3 mL of a 1:1 volume ratio mixture of dichloromethane and ethanol. The image acquisition device 250 slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 does not capture the appearance of colloidal rings in the stationary phase, the eluted fraction is aromatic hydrocarbon, which is collected in the second collection bottle 2422.

[0153] The solvent in the two extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the two extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbon WA and aromatic hydrocarbon WB were recorded.

[0154] Finally, the weights were measured: WA = 0.0775g and WB = 0.0182g.

[0155] The yield calculation formula is as follows:

[0156] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0157] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0158] Calculations showed that the refined oil sample No. 2 had a WA% of 80.98% and a WB% of 19.02%.

[0159] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 6 below.

[0160] Table 6. Hydrocarbon composition analysis results of the distillate of refined oil sample No. 2.

[0161]

[0162]

[0163] Example 7: The refined oil sample No. 2 was poured into the sample tube 223 in the first sample tray assembly 220a. The automatic extraction instrument control panel 400 was started. The temperature of the heating plate 222 was set to 60°C on the control panel 400. The quantitative needle 112 drew in 0.1g of sample. The volumetric needle 122 drew in the following volumes of the first solvent n-pentane: 1mL, 1mL, and 4mL, respectively. The volume of the second solvent dichloromethane: 1mL and 5mL, respectively. The volume of the third solvent (a 1:1 mixture of dichloromethane and ethanol): 5mL and 5mL, respectively. When the oil melts into a liquid, click to start automatic extraction. The quantitative needle 112 in the sample injection device 100 will draw 0.1g of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 will add 1mL of the first solvent, n-pentane, into the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 will draw another 1mL of n-pentane and add it to the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b will be drawn into the rinsed extraction column 232 by the volume-dilution needle 122. This process is repeated using 4mL of the same solvent. The stationary phase is rinsed with n-pentane and 1 mL of dichloromethane. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. The stationary phase is then eluted with 5 mL of dichloromethane. The multi-port valve 243 is switched to outlet b. When the dichloromethane has completely entered the stationary phase, the solid phase extraction column 232 is rinsed with 5 mL of a 1:1 volume ratio mixture of dichloromethane and ethanol. The image acquisition device 250 slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 does not capture the appearance of colloidal rings in the stationary phase, the eluted fraction is aromatic hydrocarbon, which is collected in the second collection bottle 2422.

[0164] The solvent in the two extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the two extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbon WA and aromatic hydrocarbon WB were recorded.

[0165] Finally, the weights were measured: WA = 0.0749g and WB = 0.0196g.

[0166] The yield calculation formula is as follows:

[0167] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0168] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0169] Calculations showed that the refined oil sample No. 2 had a WA% of 79.26% and a WB% of 20.74%.

[0170] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 7 below.

[0171] Table 7. Hydrocarbon composition analysis results of the distillate of refined oil sample No. 2.

[0172]

[0173]

[0174] Example 8: Pour the refined oil sample No. 2 into the sample tube 223 in the first sample tray assembly 220a, start the automatic extraction instrument control panel 400, set the temperature of the heating plate 222 to 60°C on the control panel 400, draw in 0.2g of sample with the quantitative needle 112, and draw in the following volumes of the first solvent n-pentane with the volume-depleting needle 122: 2mL, 2mL, and 5mL respectively; the following volumes of the second solvent dichloromethane with the volume: 2mL and 3mL respectively; and the following volumes of the third solvent (a 1:1 mixture of dichloromethane and ethanol with a volume ratio of 3mL and 3mL respectively). When the oil melts into a liquid, click to start automatic extraction. The quantitative needle 112 in the injection device 100 will draw 0.2g of sample from the sample tube 223 of the first sample tray assembly 220a and place it into the sample tube 223 of the second sample tray assembly 220b. Then, the volume-dilution needle 122 will add 2mL of the first solvent, n-pentane, into the sample tube 223 of the second sample tray assembly 220b. After complete dissolution, the volume-dilution needle 122 will draw another 2mL of n-pentane and add it into the extraction column 232 to rinse the extraction column 232. Then, the dissolved heavy oil in the sample tube 223 of the second sample tray assembly 220b will be drawn into the rinsed extraction column 232 by the volume-dilution needle 122. This process is repeated 5mL at a time. The stationary phase is rinsed with n-pentane and 2 mL of dichloromethane. At this time, the multi-port valve 243 is switched to outlet a to elute the adsorbed saturated hydrocarbon fraction, which is collected in the first collection bottle 2421. The stationary phase is then eluted with 5 mL of dichloromethane. The multi-port valve 243 is switched to outlet b. When the dichloromethane has completely entered the stationary phase, the solid phase extraction column 232 is rinsed with 3 mL of a 1:1 volume ratio mixture of dichloromethane and ethanol. The image acquisition device 250 gradually slides down along the drive component 211 to monitor and identify the color and position of the colloidal rings in the extraction column 232. When the image acquisition device 250 does not capture the appearance of colloidal rings in the stationary phase, the eluted fraction is aromatic hydrocarbon, which is collected in the second collection bottle 2422.

[0175] The solvent in the two extraction collection flasks 242 was evaporated in a water bath at 80℃. Then, the two extraction collection flasks 242 were placed in an oven, heated for 10 minutes, cooled for 10 minutes, weighed, and recorded. The process was repeated until the loss from two consecutive weighings was less than 20 mg. The mass of saturated hydrocarbon WA and aromatic hydrocarbon WB were recorded.

[0176] Finally, the weights were measured: WA = 0.0724g and WB = 0.0224g.

[0177] The yield calculation formula is as follows:

[0178] The content of saturated hydrocarbon fraction in the sample, WA% = WA / (WA+WB+WC)×100%;

[0179] The content of aromatic fraction in the sample, WB% = WB / (WA+WB+WC)×100%;

[0180] Calculations showed that the refined oil sample No. 2 had a WA% of 76.37% and a WB% of 23.63%.

[0181] Then, 1 mL of n-hexane was added to the first collection bottle 2421, and 1 mL of dichloromethane was added to the second collection bottle 2422. The dissolved saturated hydrocarbons and aromatics were then analyzed using a gas chromatography-mass spectrometry (GC-MS) instrument. The results are shown in Table 8 below.

[0182] Table 8. Hydrocarbon composition analysis results of the distillate of refined oil sample No. 2.

[0183]

[0184]

[0185] The various embodiments or implementation methods described in this specification are presented in a progressive manner. Each embodiment focuses on the differences from other embodiments, and the same or similar parts between the embodiments can be referred to each other.

[0186] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with an embodiment or example is included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0187] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. An automated extraction and separation system, characterized in that, include: The sample injection device includes a retractable metering device and a retractable container, the metering device being used to extract the sample by weight and the container being used to extract the solvent by volume. The control panel is electrically connected to both the injection device and the extraction device, and is used to control the injection device and the extraction device. An extraction apparatus includes a frame and at least one sample plate assembly, an extraction plate assembly, a collection plate assembly, and an image acquisition device mounted on the frame; the sample plate assembly is used to dissolve the sample, the extraction plate assembly is used to separate the sample into different products, the collection plate assembly is used to collect the separated products, and the image acquisition device is used to acquire image information from the extraction plate assembly. The liquid addition device includes multiple solvent bottles, which are fixedly mounted on a frame below the injection device for adding solvent to the extraction disk assembly.

2. The automatic extraction and separation system according to claim 1, characterized in that, The collection tray assembly includes a collection tray and at least three collection bottles, the collection bottles being placed on the collection tray; The collecting tray assembly and the extraction tray assembly are connected by a multi-way valve, which transports the different products separated by the extraction tray assembly to different collecting containers.

3. The automatic extraction and separation system according to claim 2, characterized in that, The extraction disc assembly separates up to three products, the collection disc assembly is provided with at least three collection bottles, and the multi-way valve is a four-way valve that delivers the three products to the three collection bottles respectively.

4. The automated extraction and separation system according to any one of claims 1-3, characterized in that, The image acquisition device is mounted on the frame via a drive unit, which drives the image acquisition device to move up and down along the height direction of the extraction disc assembly.

5. The automated extraction and separation system according to any one of claims 1-3, characterized in that, The extraction disk assembly includes an extraction disk and multiple extraction columns, with the extraction columns placed on the extraction disk.

6. The automated extraction and separation system according to claim 5, characterized in that, The bottom end of the extraction column is provided with an extraction port, which is connected to a control valve, and the control valve is connected to the control panel circuit.

7. The automated extraction and separation system according to claim 6, characterized in that, The extraction column includes a column body and a column head, the column head being detachably connected to the bottom end of the column body, and the control valve being connected to the column head.

8. The automated extraction and separation system according to any one of claims 1-3, characterized in that, The sample tray assembly includes a sample tray, a heating plate, and multiple sample tubes. The sample tubes are placed on the sample tray, and the heating plate is located at the bottom of the sample tray.

9. The automated extraction and separation system according to any one of claims 1-3, characterized in that, The extraction device includes a first sample tray assembly and a second sample tray assembly. The first sample tray assembly is used to melt the sample, and the second sample tray assembly is used to store a preset weight of sample and continue to dissolve the sample.

10. The automated extraction and separation system according to claim 9, characterized in that, The first sample tray assembly and the second sample tray assembly are sequentially arranged on the same side of the extraction tray assembly.

11. An automated extraction and separation method, applied to the automated extraction and separation system according to any one of claims 1-10, characterized in that, The automated extraction and separation method includes: The sample is extracted into the sample tray assembly of the extraction device by controlling the metering device through the control panel, and the sample is heated by the sample tray assembly to melt the sample. Different solvents are sequentially added to the extraction disk assembly through a fixed container to separate the stationary phase in the sample into different products, and the different products are collected in the collection disk assembly of the extraction device; wherein, the image information of the stationary phase is acquired by the image acquisition device in the extraction device to determine the separated products.

12. The automated extraction and separation method according to claim 11, characterized in that, The extraction disk assembly includes an extraction disk and multiple extraction columns. After the sample is injected into the extraction columns, the following steps are taken: The first solvent and the second solvent are added sequentially to the extraction column using the fixed container to separate the first product from the stationary phase, and the first product is collected in the first collection bottle of the collection tray assembly; The second solvent and the third solvent are sequentially added to the stationary phase using the fixed container. When the image acquisition device detects that the colloidal ring in the stationary phase has moved to the target position, the second product in the stationary phase is separated and collected in the second collection bottle in the collection tray assembly. The third solvent is added to the stationary phase using the fixed container to separate the third product from the stationary phase, and the third product is collected in the third collection bottle of the collection tray assembly.

13. The automated extraction and separation method according to claim 12, characterized in that, The extraction port at the bottom of the extraction column is connected to a control valve, and a four-way valve is connected between the collection tray assembly and the control valve. During the separation of the first product, the control valve is opened, and the four-way valve connects the extraction column and the first collection bottle; During the separation of the second product, the control valve is opened, and the four-way valve is switched to connect the extraction column and the second collecting bottle; When the image acquisition device detects that the gel ring has moved to the target position, the control valve first closes, and the four-way valve switches to connect the extraction column and the third collection bottle, and then the control valve opens.

14. The automated extraction and separation method according to claim 12, characterized in that, The image acquisition device captures the movement of the gelatinous ring to the target position, including: The image acquisition device captures the colloidal ring moving downwards to the bottom of the extraction column.

15. The automated extraction and separation method according to claim 12, characterized in that, The extraction device includes a first sample tray assembly and a second sample tray assembly. Before injecting the sample into the extraction tray assembly, the following steps are included: The sample is heated using the first sample tray assembly to melt it; A preset weight of sample is extracted using the metering device and injected into the second sample pan assembly. The first solvent is then added to the second sample pan assembly using the metering container to fully dissolve the sample.

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