CN112816313A - Device and method for digesting, separating and extracting micro-plastics in soil - Google Patents

Device and method for digesting, separating and extracting micro-plastics in soil Download PDF

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CN112816313A
CN112816313A CN202110213168.0A CN202110213168A CN112816313A CN 112816313 A CN112816313 A CN 112816313A CN 202110213168 A CN202110213168 A CN 202110213168A CN 112816313 A CN112816313 A CN 112816313A
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flotation
digestion
liquid
unit
soil
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徐笠
李芳�
陆安祥
陈早艳
付海龙
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Beijing Academy of Agriculture and Forestry Sciences
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Beijing Research Center For Agricultural Standards and Testing
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning

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  • General Health & Medical Sciences (AREA)
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  • Molecular Biology (AREA)
  • Processing Of Solid Wastes (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

The invention provides a device and a method for digesting, separating and extracting micro-plastics in soil integrally. The device integrates the processes of soil pre-digestion and micro-plastic separation into one device, and overcomes the defects of tedious and time-consuming extraction of micro-plastic, low efficiency and low recovery rate in the soil in the prior art.

Description

Device and method for digesting, separating and extracting micro-plastics in soil
Technical Field
The invention belongs to the technical field of solid waste treatment, and relates to a device and a method for digesting, separating and extracting micro-plastics in soil.
Background
Plastic products are widely used due to their low cost, lightness and plasticity, and the yield of plastics is expected to reach 330 hundred million tons in 2050. The recovery rate of the plastic is low, and the plastic entering the environment can be further broken and cracked into micro plastic through long-term physical, chemical and biological effects. Micro-plastic refers to plastic fibers, chips, granules, etc. having a particle size of less than 5 mm. The micro plastic has the characteristics of light weight, small particle size, large quantity, difficult degradation and the like, and is widely applied to oceans, land water areas and soil ecosystems. Micro-plastic contamination has become a global environmental problem and is one of the research hotspots of environmental science. Currently, much of the research on the environmental processes and ecological risks of micro-plastics is focused on aquatic environments. Land is the source of plastic production and is also an important collection area, and the micro-plastics released to the soil each year may be 4-23 times that of the ocean. Although more and more research has begun to focus on the terrestrial environment in the last two years, the research of micro-plastics in soil is still less and still more attention needs to be paid.
Patent CN107553776B discloses a manual extraction method of micro-plastics based on a manual extraction device of micro-plastics, in particular to a manual extraction device of micro-plastics, which comprises a separation barrel, a connecting barrel and a mixing barrel which are sequentially connected from top to bottom, wherein the separation barrel, the connecting barrel and the mixing barrel are integrally formed into a shell structure with only one opening at the top; a valve body assembly used for controlling whether the fluid flows is arranged in the connecting cylinder; a filter screen for filtering micro plastic is arranged above or below the valve body assembly; the wall of the mixing barrel is provided with a vent hole for gas to flow in. The method comprises the steps of sampling in a specified area of a coastal zone, taking the sampled area back and drying the area; and (3) putting the sample and the separation liquid into the extraction device, ventilating, adding liquid and the like, pouring out the precipitated micro plastic and drying. However, this patent does not deal with the treatment of organic impurities in the micro-plastic, which are embedded in the micro-plastic and easily cause the agglomeration of the micro-plastic, thereby affecting the separation of the micro-plastic, so this micro-plastic extraction device and method cannot effectively improve the recovery rate of the micro-plastic.
Patent CN111426545A discloses a method for rapidly separating micro-plastics in soil, which comprises the following steps: carrying out digestion, density separation flotation and oxidation digestion treatment on a soil sample; the former digestion is 30% H2O2Digesting the soil sample at 65-75 ℃ by using the oxidant until the color of the soil sample is changed into whiteOr the grey ends. Although the method can partially remove organic impurities in the soil by performing pre-digestion on the soil before the micro-plastic is separated, the separation efficiency is improved to a certain extent, no effective device is disclosed for rapidly and efficiently extracting the micro-plastic.
In conclusion, it is an urgent need to develop a device and method for separating micro-plastic from soil with simple operation, high recovery rate, and high speed and efficiency.
Disclosure of Invention
The invention aims to provide a device and a method for integrating digestion, separation and extraction of micro-plastics in soil.
The invention provides a device for digesting, separating and extracting micro-plastics in soil, which comprises a digestion flotation unit, a flotation liquid injection unit and a filtering unit, wherein the flotation liquid injection unit is detachably arranged above the digestion flotation unit,
a digestion flotation unit: the device is used for digesting the soil in advance to remove organic impurities in the soil, and then separating micro plastics in the soil by flotation;
a flotation solution injection unit: injecting a flotation solution into the digestion flotation unit by pressurization;
a filtering unit: used for filtering the micro plastic after flotation separation.
Further, in the digestion flotation device, the digestion flotation unit comprises an outer cylinder, a digestion flotation pool and a magnetic stirring and heating device,
the outer barrel and the digestion flotation tank are respectively containers with open upper parts, the digestion flotation tank is accommodated in the outer barrel, the bottom of the digestion flotation tank and the bottom of the outer barrel can be connected through welding or integrally formed, cooling water can be introduced into an accommodating space between the side wall of the digestion flotation tank and the side wall of the outer barrel, and a discharge port is formed in the lower part of the outer wall of the outer barrel;
the magnetic stirring and heating device is arranged below the outer barrel and used for heating and uniformly stirring the reaction materials in the digestion flotation pool.
Further, the flotation liquid injection unit comprises an air blowing pump, an air inlet pipe and a liquid adding pool,
the upper part of the liquid adding pool is provided with a sealing opening, the sealing opening is provided with a sealing cover, and the sealing cover is connected with the air-blowing pump through the air inlet pipe and is used for pressurizing and guiding the gas in the air-blowing pump into the liquid adding pool;
a liquid outlet is formed in the bottom of the liquid adding pool, extends out of the bottom of the liquid adding pool, is communicated into the digestion flotation unit, and is used for injecting the flotation liquid in the liquid adding pool into the digestion flotation pool below the liquid adding pool;
the inside in liquid feeding pond is equipped with borosilicate baffle for the short-term stay of flotation solution, the high Peng silicon baffle is located directly over the liquid outlet, with the liquid outlet remains the certain distance, the diameter of borosilicate baffle with the internal diameter in liquid feeding pond is equal.
Further, the bottom outer diameter of the flotation liquid injection unit is smaller than the upper open outer diameter of the digestion flotation unit, so that the flotation liquid injection unit is nested right at the upper open of the digestion flotation unit.
Furthermore, the filter unit includes funnel, buchner flask, rubber tube and aspiration pump, the funnel sets up buchner flask top, the below of funnel is equipped with the filter membrane, is used for collecting the micro-plastics, the buchner flask pass through the rubber tube with the aspiration pump is connected.
The invention also provides a method for integrally digesting, separating and extracting the micro-plastics in the soil by using the device, which comprises the following steps:
s1: digestion: putting soil into the digestion flotation pool, adding a Fenton reagent, digesting at 50-70 ℃ under the action of the magnetic heating and stirring device, and simultaneously introducing cooling water into an accommodating space between the side wall of the digestion flotation pool and the side wall of the outer barrel to cool the digestion reaction;
s2: flotation: after digestion is finished, draining the cooling water, adding a flotation solution into the digestion flotation pool according to the amount of soil, uniformly stirring, and standing until materials in the digestion flotation pool are divided into an upper non-precipitation layer and a lower precipitation layer, wherein the non-precipitation layer contains micro plastic particles;
s3: separation: installing the flotation liquid injection unit above the digestion flotation unit, and then adding flotation liquid into the flotation liquid injection unit, wherein the flotation liquid temporarily stays on the high borosilicate baffle; after the sealing cover is covered, the air blowing pump is started, flotation liquid can be injected into the flotation digestion tank from the liquid outlet, and along with the addition of the flotation liquid, a non-precipitation layer can overflow to the accommodating space between the side wall of the digestion flotation tank and the side wall of the outer cylinder together with micro plastic;
s4: and (3) filtering: the non-precipitation layer containing the plastic particles overflowing into the accommodating space in the step S3 flows into the filtering unit for filtering, so as to separate the micro plastic from the flotation solution.
Further, the digestion temperature is preferably 60 ℃.
Further, in step S2, the mass ratio of the soil to the flotation solution is 1: 5.
Further, in step S4, the non-precipitated layer flows out of the discharge port of the digestion flotation unit, into the filtration unit, and into the funnel, when the suction pump is activated to pump off the flotation solution, and finally the micro-plastic will remain on the filter membrane.
Further, the pore size of the filter membrane is 5 um.
Further, the density of the flotation solution is not less than 1.50g/cm3(ii) a The solute of the flotation solution is zinc chloride.
Further, the recovery of the micro-plastic is > 85%.
The invention has the following beneficial technical effects:
1. the invention adopts an integrated device of digestion, flotation and separation to carry out digestion and separation on soil micro-plastics, and organically integrates the digestion and the flotation for the first time, thereby avoiding the interference caused in the experimental process, especially the influence of the micro-plastics in the atmosphere on the experiment;
2. fenton reagent digestion is the best method in all digestion reagents at present, and the technical bottleneck is that no device is used for Fenton reagent digestion well at present.
Detailed Description
The invention is illustrated in detail below with reference to examples:
as shown in figure 1, the device for digesting, separating and extracting micro-plastics in soil of the invention comprises a digestion flotation unit, a flotation liquid injection unit and a filtering unit, wherein the flotation liquid injection unit is detachably arranged above the digestion flotation unit,
a digestion flotation unit: the device is used for digesting the soil in advance to remove organic impurities in the soil, and then separating micro plastics in the soil by flotation;
a flotation solution injection unit: injecting a flotation solution into the digestion flotation unit by pressurization;
a filtering unit: used for filtering the micro plastic after flotation separation.
Wherein, in the digestion flotation device, the digestion flotation unit comprises an outer cylinder 7, a digestion flotation pool 15 and a magnetic stirring and heating device 13,
the outer barrel 7 and the digestion flotation tank 15 are respectively containers with open upper parts, the digestion flotation tank 15 is accommodated in the outer barrel 7, the bottom of the digestion flotation tank 15 and the bottom of the outer barrel 7 can be connected by welding or integrally formed, cooling water can be introduced into an accommodating space between the side wall of the digestion flotation tank 15 and the side wall of the outer barrel 7, and a discharge port 8 is arranged at the lower part of the outer wall of the outer barrel 7;
the magnetic stirring and heating device 13 is arranged below the outer cylinder 7 and is used for heating and uniformly stirring the reaction materials in the digestion flotation pool 15.
The flotation liquid injection unit comprises an air blowing pump 1, an air inlet pipe 2 and a liquid adding pool 4,
the upper part of the liquid adding pool 4 is provided with a sealing port 14, the sealing port 14 is provided with a sealing cover 3, and the sealing cover 3 is connected with the air-blowing pump 1 through an air inlet pipe 2 and is used for pressurizing and guiding the gas in the air-blowing pump 1 into the liquid adding pool 4;
a liquid outlet 6 is arranged at the bottom of the liquid adding pool 4, the liquid outlet 6 extends out from the bottom of the liquid adding pool 4 and is communicated into the digestion flotation unit for injecting the flotation liquid in the liquid adding pool 4 into a digestion flotation pool 15 positioned below;
the inside in liquid feeding pond 4 is equipped with borosilicate baffle 5 for the short duration of flotation solution stops, and high Peng silicon baffle 5 is located liquid outlet 6 directly over, keeps the certain distance with liquid outlet 6, and the diameter of borosilicate baffle 5 is equal with the internal diameter in liquid feeding pond 4.
Further, the bottom outer diameter of the flotation liquid injection unit is smaller than the upper open outer diameter of the digestion flotation unit, so that the flotation liquid injection unit is just nested in the upper open of the digestion flotation unit.
The filter unit comprises a funnel 9, a suction flask, a rubber tube 11 and an air pump 12, wherein the funnel 9 is arranged above the suction flask 16, a filter membrane 10 is arranged below the funnel 9 and used for collecting micro-plastic, and the suction flask 16 is connected with the air pump 12 through the rubber tube 11.
The method for implementing the integral digestion and separation extraction of the micro-plastics in the soil by using the device comprises the following steps:
s1: digestion: putting soil into a digestion flotation pool 15, adding a Fenton reagent, digesting at 50-70 ℃ under the action of a magnetic heating and stirring device 13, and simultaneously introducing cooling water into an accommodating space between the side wall of the digestion flotation pool 15 and the side wall of the outer barrel 7 to cool the digestion reaction;
s2: flotation: after digestion is finished, draining cooling water, adding a flotation solution into the digestion flotation pool 15 according to the amount of soil, uniformly stirring, and standing until materials in the digestion flotation pool 15 are divided into an upper non-precipitation layer and a lower precipitation layer, wherein the non-precipitation layer contains micro plastic particles;
s3: separation: installing a flotation liquid injection unit above the digestion flotation unit, then adding flotation liquid into the flotation liquid injection unit, and temporarily stopping the flotation liquid on the high borosilicate baffle 5; after the sealing cover 3 is covered, the air blowing pump 1 is started, the flotation liquid can be injected into the digestion flotation tank 15 from the liquid outlet 6, and along with the addition of the flotation liquid, a non-precipitation layer can overflow into the accommodating space between the side wall of the digestion flotation tank 15 and the side wall of the outer cylinder 7 together with the micro-plastic;
s4: and (3) filtering: the non-precipitation layer containing the plastic particles overflowing into the accommodating space in the step S3 flows into the filtering unit for filtering, so that the micro plastic and the flotation solution are separated.
In this example, in step S2, the mass ratio of the soil to the flotation solution was 1: 5.
The density of the flotation solution is not less than 1.50g/cm3(ii) a The solute of the flotation solution is zinc chloride.
The recovery of the final microplastic was > 85% using the apparatus of this example.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, but any modifications or equivalent variations made according to the technical spirit of the present invention are still within the scope of the present invention as claimed.

Claims (9)

1. A digestion, separation and extraction integrated device for micro-plastics in soil is characterized by comprising a digestion flotation unit, a flotation liquid injection unit and a filtering unit, wherein the flotation liquid injection unit is detachably arranged above the digestion flotation unit,
a digestion flotation unit: the device is used for digesting the soil in advance to remove organic impurities in the soil, and then separating micro plastics in the soil by flotation;
a flotation solution injection unit: injecting a flotation solution into the digestion flotation unit by pressurization;
a filtering unit: used for filtering the micro plastic after flotation separation.
2. The apparatus according to claim 1, characterized in that the counteracting flotation unit comprises an outer cylinder (7), a counteracting flotation cell (15) and a magnetic stirring and heating device (13),
the outer barrel (7) and the digestion flotation tank (15) are respectively containers with the upper parts open, the digestion flotation tank (15) is accommodated in the outer barrel (7), the bottom of the digestion flotation tank (15) and the bottom of the outer barrel (7) can be connected through welding or integrally formed, cooling water can be introduced into an accommodating space between the side wall of the digestion flotation tank (15) and the side wall of the outer barrel (7), and a discharge port (8) is formed in the lower part of the outer wall of the outer barrel (7);
the magnetic stirring and heating device (13) is arranged below the outer barrel (7) and is used for heating and uniformly stirring the reaction materials in the digestion flotation pool (15).
3. The device according to claim 2, characterized in that the flotation liquid injection unit comprises an air blowing pump (1), an air inlet pipe (2) and a liquid adding tank (4),
the upper part of the liquid adding pool (4) is provided with a sealing opening (14), the sealing opening (14) is provided with a sealing cover (3), and the sealing cover (3) is connected with the air blowing pump (1) through the air inlet pipe (2) and is used for pressurizing and guiding the gas in the air blowing pump (1) into the liquid adding pool (4);
a liquid outlet (6) is formed in the bottom of the liquid adding pool (4), the liquid outlet (6) extends out of the bottom of the liquid adding pool (4) and is communicated into the digestion flotation unit, and the liquid outlet is used for injecting the flotation liquid in the liquid adding pool (4) into the digestion flotation pool (15) located below;
the inside in liquid feeding pond (4) is equipped with borosilicate baffle (5) for the short duration of flotation solution stops, Ganpeng silicon baffle (5) are located directly over liquid outlet (6), with liquid outlet (6) remain the certain distance, the diameter of borosilicate baffle (5) with the internal diameter of liquid feeding pond (4) is equivalent.
4. The apparatus according to any one of claims 1 to 3, wherein the bottom outer diameter of the flotation liquid priming unit is smaller than the upper open outer diameter of the counteracting flotation unit, such that the flotation liquid priming unit nests right at the upper open end of the counteracting flotation unit.
5. Device according to any one of claims 1 to 4, the filtration unit comprising a funnel (9), a suction flask (16), a rubber tube (11) and a suction pump (12), the funnel (9) being arranged above the suction flask (16), a filter membrane (10) being arranged below the funnel (9) for collecting the microplastic material, the suction flask (16) being connected to the suction pump (12) via the rubber tube (11).
6. A method for the integrated digestion and separation and extraction of micro-plastics in soil by means of a device according to any one of claims 1 to 5, characterized in that it comprises the following steps:
s1: digestion: putting soil into the digestion flotation pool (15), adding a Fenton reagent, digesting at 50-70 ℃ under the action of the magnetic heating and stirring device (13), and simultaneously introducing cooling water into an accommodating space between the side wall of the digestion flotation pool (15) and the side wall of the outer barrel (7) to cool a digestion reaction;
s2: flotation: after digestion is finished, draining the cooling water, adding a flotation solution into the digestion flotation pool (15) according to the amount of soil, uniformly stirring, and standing until materials in the digestion flotation pool (15) are divided into an upper non-precipitation layer and a lower precipitation layer, wherein the non-precipitation layer contains micro plastic particles;
s3: separation: installing the flotation liquid injection unit above the digestion flotation unit, and then adding flotation liquid into the flotation liquid injection unit, wherein the flotation liquid temporarily stays on the high borosilicate baffle (5); after the sealing cover (3) is covered, the air blowing pump (1) is started, the flotation liquid can be injected into the digestion flotation tank (15) from the liquid outlet (6), and along with the addition of the flotation liquid, a non-precipitation layer can overflow to the accommodating space between the side wall of the digestion flotation tank (15) and the side wall of the outer barrel (7) together with the micro plastic;
s4: and (3) filtering: the non-precipitation layer containing the plastic particles overflowing into the accommodating space in the step S3 flows into the filtering unit for filtering, so as to separate the micro plastic from the flotation solution.
7. The method of claim 6, wherein in step S2, the mass ratio of the soil to the flotation solution is 1: 5.
8. The method of claim 7, wherein the density of the flotation solution is not less than 1.50g/cm3(ii) a The solute of the flotation solution is zinc chloride.
9. The method of claim 8, wherein the recovery of the micro plastic is > 85%.
CN202110213168.0A 2021-02-26 2021-02-26 Device and method for digesting, separating and extracting micro-plastics in soil Pending CN112816313A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113075160A (en) * 2021-03-24 2021-07-06 浙江工业大学 Method for rapidly extracting and analyzing micro-plastics in soil based on density separation method
CN113640084A (en) * 2021-08-20 2021-11-12 北京大学 Detection method of farmland soil micro-plastic
CN114018659A (en) * 2021-09-24 2022-02-08 佛山科学技术学院 Soil micro-plastic separation device
CN114441428A (en) * 2022-01-14 2022-05-06 常州大学 Metal material hydrogen sulfide corrosion experiment device
CN114459870A (en) * 2022-02-11 2022-05-10 扬州大学 Efficient and economical soil micro-plastic separation and purification device and method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113075160A (en) * 2021-03-24 2021-07-06 浙江工业大学 Method for rapidly extracting and analyzing micro-plastics in soil based on density separation method
CN113640084A (en) * 2021-08-20 2021-11-12 北京大学 Detection method of farmland soil micro-plastic
CN114018659A (en) * 2021-09-24 2022-02-08 佛山科学技术学院 Soil micro-plastic separation device
CN114441428A (en) * 2022-01-14 2022-05-06 常州大学 Metal material hydrogen sulfide corrosion experiment device
CN114459870A (en) * 2022-02-11 2022-05-10 扬州大学 Efficient and economical soil micro-plastic separation and purification device and method

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