Rapid extraction and purification device for soil organic pollutants

Abstract

The invention provides a rapid extraction and purification device for soil organic pollutants, and belongs to the technical field of soil analysis and detection. Comprising a soil crushing unit, a liquid phase extraction unit and a solid phase extraction unit for purifying extracted organic matters, according to the device, the organic pollutants are transferred into water or an organic phase through the liquid phase extraction unit, the organic pollutants are transferred into an organic solvent by directly utilizing portable gas chromatography, portable gas chromatography-mass spectrometry and other devices for sample introduction after being enriched through the solid phase microextraction sample introduction needle, and the solid phase extraction unit is utilized for on-site purification treatment. By means of the technical advantages of multi-mode extraction, efficient enrichment, on-site purification and portable combination, the defects that in traditional soil organic pollutant analysis, the process is tedious, consumed time is long, and dependence is made on a laboratory are overcome, and the method is particularly suitable for environment emergency, pollution investigation and field monitoring scenes.

Description

Technical Field

[0001] The invention belongs to the technical field of soil analysis and detection, and in particular is a device for rapid extraction and purification of soil organic pollutants. Background Art

[0002] Soil organic pollutants refer to organic compounds that enter the soil environment, including chlorinated hydrocarbons, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, pesticides, petroleum hydrocarbons, etc. These pollutants are toxic, persistent and bioaccumulative, and will pose a serious threat to soil ecosystems, groundwater and human health. For example, polycyclic aromatic hydrocarbons are a type of environmental organic pollutant that is easily distributed in soil organic matter. The International Agency for Research on Cancer has listed some polycyclic aromatic hydrocarbons as potential human carcinogens.

[0003] In the on-site emergency detection scenario of soil pollution, portable gas chromatographs and gas chromatography-mass spectrometry (GC-MS) have become ideal on-site detection equipment due to their rapid analysis capabilities. However, due to the complexity of soil pretreatment steps and the difficulty of on-site extraction of target pollutants (especially high-boiling point organic pollutants), this type of technology has not yet been effectively applied to the actual analysis of organic pollutants in soil. Existing soil organic pollutant extraction and purification devices generally have the defect of insufficient flexibility and require a lot of manpower and time in the laboratory. Not only can they not meet the urgent need of on-site emergency detection for "rapid acquisition of analyzable samples", but also due to the bottleneck problem in the pre-treatment link, it is difficult to improve the analytical recovery rate of portable detection equipment, which seriously restricts the application of on-site real-time detection technology in soil pollution assessment.

[0004] Therefore, there is an urgent need to develop a device that can specifically solve the problem of rapid extraction of high-boiling-point organic pollutants in soil. By optimizing the pretreatment process, the efficiency of introducing target pollutants into portable gas chromatography or gas chromatography-mass spectrometry can be improved, providing efficient and reliable technical support for on-site emergency detection. Summary of the Invention

[0005] In response to the above-mentioned problems, the present invention provides a device for rapid extraction and purification of soil organic pollutants.

[0006] The technical solution of the present invention is: a rapid extraction and purification device for soil organic pollutants, comprising a purification body with an addition port at the upper end, a soil crushing unit disposed in the purification body and connected to the bottom end of the addition port, a liquid extraction unit, a solid phase extraction unit connected to the liquid extraction unit, and a purification unit;

[0007] The side wall of the purification body is provided with a box door, and the solid phase extraction unit and the purification unit are respectively connected to a waste liquid storage box; the bottom end of the soil crushing unit is provided with a temporary storage tray;

[0008] The liquid phase extraction unit includes a vertical mounting rod connected to the bottom end of the temporary storage tray, a plurality of extraction cylinders distributed circumferentially around the vertical mounting rod, a first addition ring and a second addition ring in which the extraction cylinders are sleeved, a first addition cylinder connected to the first addition ring, and a second addition cylinder connected to the second addition ring;

[0009] Several addition branches are provided through the contact points between the first addition ring and the second addition ring and each extraction cylinder. A discharge port and a microwave generator are provided at the bottom of the temporary storage tray corresponding to the upper end of each extraction cylinder. The upper side wall of each extraction cylinder is connected to the solid phase extraction unit and the purification unit through a discharge pipe, and a heater is provided on the inner wall of the extraction cylinder.

[0010] Furthermore, a liquid level sensor is provided in the waste liquid storage tank, and electronic flow meters and liquid pumps are provided at the connections between the waste liquid storage tank, the solid phase extraction unit and the purification unit.

[0011] Description: The liquid level sensor monitors the liquid level of the two waste liquid storage tanks connected to the solid phase extraction unit and the purification unit in real time. The residual liquid in the solid phase extraction unit and the purification unit is pumped into the corresponding waste liquid storage tanks by the liquid pump. No manual operation is required, which reduces labor costs and improves process efficiency.

[0012] Furthermore, the soil crushing unit includes a crushing box which is connected to the bottom end of the addition port and is provided with a filter plate at the connection, and a heating box which is provided between the crushing box and the temporary storage tray.

[0013] Description: When the soil crushing unit treats contaminated soil, the contaminated soil is first added to the purification body through the addition port. At this time, it is first filtered and removed through the filter plate, and then the contaminated soil is crushed by the crushing box. The crushed soil falls into the heating box for heating and drying. The triple mechanism of impurity filtration + physical crushing and thermal activation significantly improves the extraction efficiency and detection accuracy of organic pollutants.

[0014] Furthermore, a gradient heating module is provided in the heating box, and the gradient heating module includes a vertical mounting frame, a first heating cover with several side walls inclined downwardly arranged on the vertical mounting frame from top to bottom, and a second heating cover arranged on the inner wall of the heating box corresponding to the lower end of each first heating cover and inclined upward. A heating plate is provided on the first heating cover, and a blanking channel is formed between the second heating cover and the corresponding first heating cover.

[0015] Description: When the crushed soil falls into the heating box, it first falls onto the first heating plate at the top, and then slides down along the side wall of the first heating plate under the action of gravity. During this process, the first heating and drying is carried out. Then, the soil falls through the edge of the first heating plate to the second heating cover at the top, and is evenly scattered onto the second heating plate through the blanking channel. Under the action of gravity, it slides down along the side wall of the second heating plate. During this process, the second heating and drying is carried out. This is repeated, and the soil is heated several times through each heating plate. Each layer of heating plate is independently temperature-controlled, so that the soil particles can be progressively dried in different temperature sections during the sliding process, and are evenly dispersed through the second heating cover between two adjacent heatings, thereby increasing the soil falling path, improving the uniformity of soil drying, and avoiding fluctuations in extraction efficiency caused by differences in local physical properties of the soil. The pores of the dried soil are open, and the extractant can directly contact the pollutant adsorption sites, thereby improving the extraction kinetics rate.

[0016] Furthermore, the first heating cover includes several support rods hinged to the outer wall of the vertical mounting frame along the circumferential direction, a mounting sleeve sleeved on the outer wall of the vertical mounting frame and located at the lower end of the support rod, and a first micro-electric telescopic rod for connecting the mounting sleeve and each support rod, the heating plate is movably connected to the upper end of each support rod, and the second heating cover is an annular structure with a downwardly inclined side wall.

[0017] Description: When it is necessary to adjust the soil sliding rate at each drop channel, the corresponding support rod is rotated by telescoping or extending the first micro-electric telescopic rod, thereby adjusting the inclination angle of the support rod to achieve the purpose of adjusting the soil sliding rate at the drop channel. The inclination angle of each layer of support rods can be controlled independently to form a gradient drying path. The upper layer is quickly dried to reduce soil caking; the lower layer is slowly dried to ensure that the moisture content meets the standard. This realizes the precise control of the soil drying process, which not only improves the drying quality and efficiency, but also lays a good foundation for the subsequent extraction process.

[0018] Furthermore, the upper ends of the heating plate and the second heating cover are both provided with a plurality of barrier strips.

[0019] Description: When the soil slides down from the upper end of the heating plate and the second heating cover, the barrier strips prevent the soil from sliding directly and quickly, so that the actual movement path of the soil on the heating plate and the second heating cover is changed from a straight line to a broken line, which prolongs the contact time with the heat source and accelerates the drying process.

[0020] Furthermore, the solid phase extraction unit includes a mounting main frame connected to the inner wall of the purification body on one side and composed of two parallel vertical mounting plates, a liquid separation box arranged between the two vertical mounting plates and whose side walls are connected to each of the extraction cylinders through the drainage pipe, a reagent temporary storage box arranged between the two vertical mounting plates and located directly below the liquid separation box, and several placement plates arranged between the reagent temporary storage box and the liquid separation box and distributed from top to bottom, each of the placement plates is provided with several placement holes, and an extraction column is placed in each of the placement holes, and a liquid separation branch pipe corresponding to the placement holes is provided at the bottom of the liquid separation box, and both ends of the placement plate can slide back and forth along the two vertical mounting plates.

[0021] Description: When the solid phase extraction unit is in use, the pollutants are transferred to the water through extraction, and the water is pumped into the separation box through the drainage pipe. At this time, one of the placement plates is slid to be located at the lower end of the separation box, and the water is discharged into the extraction columns on the placement plate through the various separation branches at the bottom of the separation box. The organic matter in the water is adsorbed by the adsorbent in the extraction column to achieve the extraction and enrichment of the organic matter. The remaining water falls into the reagent temporary storage box through the bottom of the extraction column. In order to maintain continuity, after the above-mentioned placement plate is used up, it is pushed and away from the lower end of the separation box, and then the placement plate at its lower end is pushed to be located at the separation At the lower end of the liquid tank, repeat the above extraction steps until the extraction columns on the upper ends of each placement plate are used. When the upper placement plate is working, the extraction columns of the used lower placement plate can be replaced, waste liquid can be cleaned up, etc., forming a parallel process of "processing-column replacement", shortening the overall processing cycle, and can flexibly respond to fluctuations in sample volume by increasing or decreasing the number of placement plates or adjusting the density of individual extraction columns. It breaks through the bottleneck of low single processing volume and cumbersome operation of traditional solid-phase extraction, and significantly improves the processing efficiency of the equipment while ensuring the extraction effect. It is especially suitable for the "large-scale, multi-batch, high-precision" processing requirements in rapid soil pollution detection.

[0022] Furthermore, several horizontal sliding grooves corresponding to the placement plates are provided on opposite sides of the two vertical mounting plates, and each of the horizontal sliding grooves is provided with a second micro electric telescopic rod which drives the placement plate to slide back and forth and is placed horizontally, and the distance between two adjacent horizontal sliding grooves is greater than the length of the extraction column.

[0023] Description: The two ends of the placement plate are limited by the horizontal sliding groove to improve the installation stability of the placement plate. At the same time, when the placement plate slides back and forth in the horizontal sliding groove, it is driven by the second micro-electric telescopic rod, eliminating the need for frequent manual operation and shortening the process interval time. By limiting the distance between two adjacent horizontal sliding grooves to be greater than the length of the extraction column, it is ensured that when two adjacent placement plates are placed one above the other, there will be no collision between the two adjacent extraction columns above and below, thereby improving the reliability of the solid phase extraction unit.

[0024] Furthermore, an atomizing nozzle is provided on each of the adding branches and located on the inner wall of the extraction cylinder, and the atomizing nozzle is flush with the inner wall surface of the extraction cylinder.

[0025] Description: When adding water to each extraction cylinder through the addition branch pipe on the first addition ring, or adding organic phase to each extraction cylinder through the addition branch pipe on the second addition ring, the water or organic phase is atomized by the atomizing nozzle, so that the pollutants on the surface of the soil particles can be dissolved or adsorbed into the fluid more quickly, shortening the extraction equilibrium time. By limiting the atomizing nozzle to be flush with the inner wall surface of the extraction cylinder, it is avoided that when the nozzle protrudes, the high-speed spray droplets may hit the inner wall of the extraction cylinder to form wall flow, reducing the direct impact on the inner wall of the extraction cylinder, and the droplets are more likely to adhere to the surface of the soil particles rather than run off along the wall, thereby increasing the interaction time between the fluid and the soil.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] When in use, the soil organic pollutant rapid extraction and purification device of the present invention filters and crushes the soil to be tested through the soil crushing unit to ensure the uniformity of the soil sample, reduce caking, and improve the subsequent extraction efficiency. The pretreated soil is subjected to liquid phase extraction through the liquid phase extraction unit. During liquid phase extraction, water extraction can be used and solid phase extraction can be performed in conjunction with the solid phase extraction unit, and organic phase extraction can be used and purification can be performed in conjunction with the purification unit. The dual-mode design covers most types of organic pollutants and can cope with complex pollution scenarios without changing equipment. In the liquid phase extraction process, microwave energy is directly applied to soil particles, causing molecules to generate heat through high-speed friction, quickly destroying the pollutant-soil binding bonds, and improving extraction efficiency. Through the technical advantages of multi-mode extraction, efficient enrichment, on-site purification and portable combination, the shortcomings of traditional soil organic pollutant analysis, such as complicated processes, long time consumption and laboratory dependence, are solved. It is particularly suitable for environmental emergency, pollution investigation and field monitoring scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the external overall structure of the present invention;

[0029] Figure 2 It is a schematic diagram of the internal overall structure of the present invention;

[0030] Figure 3 It is a schematic diagram of the internal structure of the heating box of the present invention;

[0031] Figure 4 It is a structural schematic diagram of the first heating cover of the present invention;

[0032] Figure 5 It is a top view of the support rods of the present invention distributed on the outer wall of the vertical mounting frame;

[0033] Figure 6 This is a top view of the heating plates of the present invention distributed on the outer wall of a vertical mounting frame;

[0034] Figure 7 is a top view of the distribution of the second heating cover and the heating plate of the present invention;

[0035] Figure 8 Schematic diagram of the internal structure of the extraction cartridge of the present invention;

[0036] Figure 9 Schematic diagram of the installation structure of the solid phase extraction unit of the present invention;

[0037] Figure 10 It is a top view of the installation of the placement plate of the present invention.

[0038] Among them, 1-purification body, 10-addition port, 11-box door, 12-waste liquid storage box, 120-liquid level sensor, 121-electronic flow meter, 122-liquid pump, 2-soil crushing unit, 20-filter plate, 21-crushing box, 22-heating box, 23-vertical mounting frame, 24-first heating cover, 240-support rod, 241-mounting sleeve, 242-first micro electric telescopic rod, 243-barrier strip, 25-second heating cover, 26-heating plate, 27-feeding channel, 3-liquid phase extraction unit, 30-temporary storage tray, 300-discharge port , 301-microwave generator, 31-vertical mounting rod, 32-extraction cylinder, 320-drain pipe, 33-first addition ring, 34-second addition ring, 35-first addition cylinder, 36-second addition cylinder, 37-addition branch pipe, 370-atomizing nozzle, 4-solid phase extraction unit, 40-vertical mounting plate, 400-horizontal sliding groove, 401-second micro electric telescopic rod, 41-mounting main frame, 42-liquid separation box, 420-liquid separation branch pipe, 43-reagent temporary storage box, 44-placement plate, 440-placement hole, 441-extraction column, 5-purification unit. DETAILED DESCRIPTION

[0039] In order to further understand the content of the present invention, the present invention is described in detail below through examples.

[0040] Example 1: Figure 1 、 2 As shown, a rapid extraction and purification device for soil organic pollutants includes a purification body 1 with an addition port 10 at the top, a soil crushing unit 2 disposed in the purification body 1 and connected to the bottom of the addition port 10, a liquid extraction unit 3, a solid phase extraction unit 4 connected to the liquid extraction unit 3, and a purification unit 5, wherein the purification unit 5 adopts existing technology, for example, a microporous filter membrane device;

[0041] The side wall of the purification body 1 is provided with a box door 11, and the solid phase extraction unit 4 and the purification unit 5 are respectively connected to the waste liquid storage box 12; the bottom end of the soil crushing unit 2 is provided with a temporary storage tray 30;

[0042] The liquid extraction unit 3 includes a vertical mounting rod 31 connected to the bottom end of the temporary storage tray 30, four extraction cartridges 32 distributed circumferentially around the vertical mounting rod 31, a first addition ring 33 and a second addition ring 34 in which each extraction cartridge 32 is nested, a first addition cartridge 35 connected to the first addition ring 33, and a second addition cartridge 36 connected to the second addition ring 34.

[0043] Three addition branches 37 are provided through the contact points between the first addition ring 33 and the second addition ring 34 and each extraction cylinder 32. A discharge port 300 and a microwave generator 301 are provided at the bottom end of the temporary storage tray 30 corresponding to the upper end of each extraction cylinder 32. The upper side wall of each extraction cylinder 32 is connected to the solid phase extraction unit 4 and the purification unit 5 through a discharge pipe 320. A heater is provided on the inner wall of the extraction cylinder 32. The microwave generator 301 and the heater both adopt existing technologies. For example, the microwave generator 301 can adopt the model M100SF-1 microwave generator. The heater is used to improve the extraction efficiency of organic pollutants in the soil by heating. The HT-12T soil organic carbon constant temperature heater can be used.

[0044] The soil crushing unit 2 includes a crushing box 21 which is connected to the bottom end of the addition port 10 and is provided with a filter plate 20 at the connection, and a heating box 22 provided between the crushing box 21 and the temporary storage tray 30. When the soil crushing unit 2 treats the contaminated soil, the contaminated soil is first added to the purification body 1 through the addition port 10. At this time, the contaminated soil is first filtered and removed by the filter plate 20, and then the contaminated soil is crushed by the crushing box 21. The crushed soil falls into the heating box 22 for heating and drying. Through the triple mechanism of impurity filtration + physical crushing and thermal activation, the extraction efficiency and detection accuracy of organic pollutants are significantly improved. Among them, the filter plate 20 adopts existing technology, for example, an existing metal woven filter plate can be used;

[0045] like Figure 3As shown, a gradient heating module is provided in the heating box 22, which includes a vertical mounting frame 23, a plurality of first heating covers 24 with downwardly inclined side walls provided on the vertical mounting frame 23 from top to bottom, and a second heating cover 25 provided on the inner wall of the heating box 22 at the lower end of each first heating cover 24 and inclined upward. A heating plate 26 is provided on the first heating cover 24, and a drop channel 27 is formed between the second heating cover 25 and the corresponding first heating cover 24. The soil is heated several times through each heating plate 26, and each layer of heating plate is independently temperature-controlled, so that the soil particles can be contacted during the sliding process. The soil is progressively dried in different temperature sections and evenly dispersed through the second heating cover 25 between two adjacent heating periods, thereby increasing the soil drop path, improving the uniformity of soil drying, and avoiding fluctuations in extraction efficiency caused by differences in local physical properties of the soil. The pores of the dried soil are open, allowing the extractant to directly contact the adsorption sites of pollutants, thereby improving the extraction kinetics rate. The heating plate 26 and the second heating cover 25 both adopt existing technologies, for example, the heating plate 26 adopts a DL-SM600 heating plate, and the second heating cover 25 adopts an existing T2 copper ring plate.

[0046] like Figure 4 、 5 As shown in Figure 6, the first heating cover 24 includes several support rods 240 hinged to the outer wall of the vertical mounting frame 23 along the circumferential direction, a mounting sleeve 241 sleeved on the outer wall of the vertical mounting frame 23 and located at the lower end of the support rod 240, and a first micro-electric telescopic rod 242 for connecting the mounting sleeve 241 and each support rod 240. The heating plate 26 is movably connected to the upper end of each support rod 240. The second heating cover 25 is an annular structure with a downwardly inclined side wall. When it is necessary to adjust the soil sliding rate at each drop channel 27, the corresponding support rod 240 is rotated by telescoping or extending the first micro-electric telescopic rod 242. The tilt angle of the support rod 240 is adjusted to adjust the sliding rate of the soil at the drop channel 27. The tilt angle of each layer of support rods 240 can be independently controlled, such as the upper layer is fast and the lower layer is slow, forming a gradient drying path. The upper layer is quickly dried to reduce soil caking; the lower layer is slowly dried to ensure that the moisture content meets the standard. The precise control of the soil drying process is realized, which not only improves the drying quality and efficiency, but also lays a good foundation for the subsequent extraction process. Among them, the first micro electric telescopic rod 242 adopts the existing technology, for example, the micro electric telescopic rod with model YFN819 can be used;

[0047] like Figure 7As shown, the heating plate 26 is provided with 35 barrier strips 243, and the upper end of the second heating cover 25 is provided with 6 barrier strips 243. When the soil slides downward from the upper ends of the heating plate 26 and the second heating cover 25, the barrier strips 243 prevent the soil from sliding directly and quickly, so that the actual movement path of the soil on the heating plate 26 and the second heating cover 25 is changed from a straight line to a broken line, thereby extending the contact time with the heat source and accelerating the drying process.

[0048] The solid phase extraction unit 4 includes a mounting main frame 41 connected to the inner wall of the purification body 1 on one side and composed of two parallel vertical mounting plates 40, a liquid separation box 42 arranged between the two vertical mounting plates 40 and connected to each extraction cylinder 32 through a drain pipe 320 on the side wall, a reagent temporary storage box 43 arranged between the two vertical mounting plates 40 and located directly below the liquid separation box 42, and three placement plates 44 arranged between the reagent temporary storage box 43 and the liquid separation box 42 and distributed from top to bottom, each placement plate 44 is provided with 15 placement holes 440, and an extraction column 441 is placed in each placement hole 440. The bottom end of the liquid separation box 42 is provided with a liquid separation branch pipe 420 corresponding to the placement hole 440. Both ends of the placement plate 44 can be Sliding back and forth along the two vertical mounting plates 40, when the upper placement plate 44 is working, the extraction column replacement, waste liquid cleaning and other operations can be carried out on the used lower placement plate 44 simultaneously, forming a parallel process of "processing-column replacement", shortening the overall processing cycle, and can flexibly respond to sample volume fluctuations by increasing or decreasing the number of placement plates 44 or adjusting the density of the extraction column 441 of a single 44, breaking through the bottleneck of low single processing volume and cumbersome operation of traditional solid-phase extraction, while ensuring the extraction effect, significantly improving the processing efficiency of the equipment, especially suitable for the "large-scale, multi-batch, high-precision" processing requirements in rapid soil pollution detection. Among them, the extraction column 441 adopts existing technology, for example, the Supelco ENVI-Chrom P series extraction column can be used.

[0049] Example 2: This example discloses a method for rapid extraction and purification of soil organic pollutants, based on a rapid extraction and purification device for soil organic pollutants in Example 1, comprising the following steps:

[0050] S1. First, add contaminated soil into the purification body 1 through the addition port 10. At this time, it is first filtered and removed by the filter plate 20, and then the contaminated soil is crushed by the crushing box 21. The crushed soil falls into the heating box 22;

[0051] S2. When the crushed soil falls into the heating box 22, it first falls onto the first heating plate 26 at the top, and then slides down along the side wall of the first heating plate 26 under the action of gravity. During this process, it is heated and dried for the first time. Then, the soil falls onto the second heating cover 25 at the top through the edge of the first heating plate 26, and is evenly scattered onto the second heating plate 26 through the blanking channel 27. Under the action of gravity, it slides down along the side wall of the second heating plate 26, and is heated and dried for the second time. This process is repeated, and the soil is heated several times by each heating plate 26, and each layer of heating plate is independently temperature-controlled.

[0052] S3. The soil processed in step S2 falls into the temporary storage tray 30 and is discharged through the discharge ports 300 at the bottom of the temporary storage tray 30. The fallen soil is then wrapped in tin foil and added to the extraction cylinders 32. At the same time, the microwave generator 301 is turned on to emit microwaves into the extraction cylinders 32.

[0053] S4. When liquid-phase extraction of soil is performed using water, the water in the first addition cylinder 35 is evenly added to the soil in each extraction cylinder 32 through the addition branch pipe 37 and mixed, thereby extracting organic matter in the soil into the water. When liquid-phase extraction of soil is performed using an organic phase, the organic phase in the second addition cylinder 36 is evenly added to the soil in each extraction cylinder 32 through the addition branch pipe 37 and mixed, thereby extracting organic matter in the soil into the organic phase.

[0054] S5. After the organic matter in the soil is extracted into the water, the water is pumped into the liquid separation box 42 through the drainage pipe 320. At this time, one of the placement plates 44 is slid so that it is located at the lower end of the liquid separation box 42. The water is discharged into the extraction columns 441 on the placement plate 44 through the various liquid separation branches 420 at the bottom end of the liquid separation box 42. The organic matter in the water is adsorbed by the adsorbent in the extraction columns 441 to achieve extraction and enrichment of the organic matter. The remaining water falls into the reagent temporary storage box 43 through the bottom end of the extraction column 441. In order to maintain continuity, after the above-mentioned placement plate 44 is used, it is pushed and away from the lower end of the liquid separation box 42. Then, the placement plate 44 at its lower end is pushed again to be located at the lower end of the liquid separation box 42, and the above-mentioned extraction steps are repeated.

[0055] S6, after the organic matter in the soil is extracted into the organic phase, the organic phase is pumped into the purification unit 5 through another drainage pipe 320 and purified;

[0056] S7. Use the water in the reagent storage box 43 and the organic phase treated by the purification unit 5 as test samples and use external detection equipment to detect them. Finally, the remaining residual liquid in the reagent storage box 43 will be discharged into the corresponding waste liquid storage box 12, and the box door 11 can be opened for cleaning.

[0057] Example 3: This example differs from Example 1 in that:

[0058] A liquid level sensor 120 is provided in the waste liquid storage tank 12. An electronic flow meter 121 and a liquid pump 122 are provided at the connection between the waste liquid storage tank 12 and the solid phase extraction unit 4 and the purification unit 5. The liquid level of the two waste liquid storage tanks 12 connected to the solid phase extraction unit 4 and the purification unit 5 is monitored in real time by the liquid level sensor 120. The residual liquid in the solid phase extraction unit 4 and the purification unit 5 is pumped into the corresponding waste liquid storage tank 12 by the liquid pump 122. No manual operation is required, which reduces labor costs and improves process efficiency. Among them, the liquid level sensor 120, the electronic flow meter 121 and the liquid pump 122 all adopt existing technologies. For example, the liquid level sensor 120 can adopt a liquid level sensor with a model number of JYB-KO-Y5, the electronic flow meter 121 can adopt a model number of SLX series electronic flow meter, and the liquid pump 122 can adopt a model number of Kamoer KLP04.

[0059] like Figure 9 、 10 As shown, three horizontal sliding grooves 400 corresponding to the placement plates 44 are provided on opposite sides of the two vertical mounting plates 40, and each horizontal sliding groove 400 is provided with a second micro-electric telescopic rod 401 that drives the placement plate 44 to slide back and forth and is placed horizontally. The distance between two adjacent horizontal sliding grooves 400 is greater than the length of the extraction column 441. The two ends of the placement plate 44 are limited by the horizontal sliding grooves 400, thereby improving the installation stability of the placement plate 44. At the same time, when the placement plate 44 slides back and forth in the horizontal sliding groove 400, it is driven by the second micro-electric telescopic rod 401, without the need for frequent manual operation, thereby shortening the process interval time. By limiting the distance between two adjacent horizontal sliding grooves 400 to be greater than the length of the extraction column 441, it is ensured that when the two adjacent placement plates 44 are placed one above the other, there will be no collision between the two adjacent extraction columns 441 above and below, thereby improving the reliability of the solid phase extraction unit 4. Among them, the second micro-electric telescopic rod 401 adopts the existing technology, for example, a micro-electric telescopic rod with model YFN819 can be used;

[0060] like Figure 8As shown, an atomizing nozzle 370 is provided on each addition branch pipe 37 and located on the inner wall of the extraction cylinder 32. The atomizing nozzle 370 is flush with the inner wall surface of the extraction cylinder 32. When water is added to each extraction cylinder 32 through the addition branch pipe 37 on the first addition ring 33, or when an organic phase is added to each extraction cylinder 32 through the addition branch pipe 37 on the second addition ring 34, the water or organic phase is atomized by the atomizing nozzle 370, so that pollutants on the surface of soil particles can be dissolved or adsorbed into the fluid more quickly, shortening the extraction equilibrium time. By limiting the atomizing nozzle 370 to be flush with the inner wall surface of the extraction cylinder 32, the high-speed spray droplets are prevented from hitting the inner wall of the extraction cylinder 32 to form wall flow when the nozzle protrudes, reducing direct impact on the inner wall of the extraction cylinder 32. The droplets are more likely to adhere to the surface of soil particles rather than flow along the wall, thereby increasing the interaction time between the fluid and the soil. The atomizing nozzle 370 adopts existing technology, for example, an atomizing nozzle model ZSTW A40 / 120 can be used.

[0061] Example 4: This example differs from Example 2 in that:

[0062] In step S5, the placement plate 44 is driven by the second micro electric telescopic rod 401 when sliding back and forth in the horizontal sliding groove 400;

[0063] In step S4 , when water is added to each extraction cylinder 32 through the addition branch pipe 37 on the first addition ring 33 , or when organic phase is added to each extraction cylinder 32 through the addition branch pipe 37 on the second addition ring 34 , the water or organic phase is atomized by the atomizing nozzle 370 .

Claims

1. A rapid extraction and purification device for soil organic pollutants, characterized in that: It comprises a purification body (1) with an addition port (10) at its upper end, a soil crushing unit (2) provided in the purification body (1) and connected to the bottom end of the addition port (10), a liquid extraction unit (3), a solid phase extraction unit (4) connected to the liquid extraction unit (3), and a purification unit (5); The side wall of the purification body (1) is provided with a box door (11); the solid phase extraction unit (4) and the purification unit (5) are respectively connected to a waste liquid storage box (12); the bottom end of the soil crushing unit (2) is provided with a temporary storage tray (30); The liquid phase extraction unit (3) comprises a vertical mounting rod (31) connected to the bottom end of the temporary storage tray (30), a plurality of extraction cylinders (32) circumferentially distributed around the vertical mounting rod (31), a first addition ring (33) and a second addition ring (34) in which each of the extraction cylinders (32) is sleeved, a first addition cylinder (35) connected to the first addition ring (33), and a second addition cylinder (36) connected to the second addition ring (34); Several addition branches (37) are provided through the contact points between the first addition ring (33) and the second addition ring (34) and each extraction cylinder (32); a discharge port (300) and a microwave generator (301) are provided at the bottom end of the temporary storage tray (30) corresponding to the upper end of each extraction cylinder (32); the upper side wall of each extraction cylinder (32) is connected to the solid phase extraction unit (4) and the purification unit (5) through a discharge pipe (320); and a heater is provided on the inner wall of the extraction cylinder (32).

2. The device for rapid extraction and purification of soil organic pollutants according to claim 1, characterized in that: A liquid level sensor (120) is provided in the waste liquid storage tank (12), and an electronic flow meter (121) and a liquid pump (122) are provided at the connection points between the waste liquid storage tank (12), the solid phase extraction unit (4) and the purification unit (5).

3. The rapid extraction and purification device for soil organic pollutants according to claim 1, characterized in that: The soil crushing unit (2) comprises a crushing box (21) which is connected to the bottom end of the addition port (10) and is provided with a filter plate (20) at the connection, and a heating box (22) which is provided between the crushing box (21) and the temporary storage tray (30).

4. The device for rapid extraction and purification of soil organic pollutants according to claim 3, characterized in that: A gradient heating module is provided in the heating box (22), and the gradient heating module comprises a vertical mounting frame (23), a plurality of first heating covers (24) with downwardly inclined side walls provided on the vertical mounting frame (23) from top to bottom, and a second heating cover (25) provided on the inner wall of the heating box (22) at the lower end corresponding to each of the first heating covers (24) and inclined upward, a heating plate (26) is provided on the first heating cover (24), and a blanking channel (27) is formed between the second heating cover (25) and the corresponding first heating cover (24).

5. The device for rapid extraction and purification of soil organic pollutants according to claim 4, characterized in that: The first heating cover (24) comprises a plurality of support rods (240) hingedly connected to the outer wall of the vertical mounting frame (23) along the circumferential direction, a mounting sleeve (241) sleeved on the outer wall of the vertical mounting frame (23) and located at the lower end of the support rods (240), and a first micro-electric telescopic rod (242) for connecting the mounting sleeve (241) and each support rod (240); the heating plate (26) is movably connected to the upper end of each support rod (240); and the second heating cover (25) is an annular structure with a downwardly inclined side wall.

6. The device for rapid extraction and purification of soil organic pollutants according to claim 5, characterized in that: The upper ends of the heating plate (26) and the second heating cover (25) are both provided with a plurality of barrier strips (243).

7. The device for rapid extraction and purification of soil organic pollutants according to claim 1, characterized in that: The solid phase extraction unit (4) comprises a mounting main frame (41) connected to the inner wall of the purification body (1) on one side and composed of two parallel vertical mounting plates (40), a liquid separation box (42) provided between the two vertical mounting plates (40) and having a side wall connected to each of the extraction cylinders (32) through the liquid discharge pipe (320), and a reagent temporary storage box (43) provided between the two vertical mounting plates (40) and located directly below the liquid separation box (42). ), a plurality of placement plates (44) are arranged between the reagent temporary storage box (43) and the liquid separation box (42) and distributed from top to bottom, each of the placement plates (44) is provided with a plurality of placement holes (440), and an extraction column (441) is placed in each of the placement holes (440). The bottom end of the liquid separation box (42) is provided with a liquid separation branch pipe (420) corresponding to the placement holes (440) one by one, and the two ends of the placement plate (44) can slide back and forth along the two vertical mounting plates (40).

8. The device for rapid extraction and purification of soil organic pollutants according to claim 7, characterized in that: A plurality of horizontal sliding grooves (400) corresponding to the placement plate (44) are provided on opposite sides of the two vertical mounting plates (40), and each of the horizontal sliding grooves (400) is provided with a second micro electric telescopic rod (401) that drives the placement plate (44) to slide forward and backward and is placed horizontally, and the distance between two adjacent horizontal sliding grooves (400) is greater than the length of the extraction column (441).

9. The device for rapid extraction and purification of soil organic pollutants according to claim 1, characterized in that: An atomizing nozzle (370) is provided on each of the adding branches (37) and located on the inner wall of the extraction cylinder (32), and the atomizing nozzle (370) is flush with the inner wall surface of the extraction cylinder (32).

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