CN109655321A - The floating and enriching device and its screening technique of micro- plastics - Google Patents
The floating and enriching device and its screening technique of micro- plastics Download PDFInfo
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- CN109655321A CN109655321A CN201811321283.4A CN201811321283A CN109655321A CN 109655321 A CN109655321 A CN 109655321A CN 201811321283 A CN201811321283 A CN 201811321283A CN 109655321 A CN109655321 A CN 109655321A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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Abstract
The invention discloses the floating and enriching devices and its screening technique of micro- plastics, basic principle is that the bubble difference of adhesion properties and highdensity flotation solution on hydrophilic and hydrophobic material can be changed based on biosurfactant to improve to the micro- plastics separating effect of high density.The device of invention includes flotation fluid liquid storage device, separating pipe, aerator and Suction filtration device, the agitation of uprising gas fortification system is generated using aerating system, minute bubbles coat micro- plastics quick separating, micro- plastics separating property is improved from spilling suitable for reading by flotation fluid systems force flotation fluid after standing.Operation is simple for the micro- flotation of Plastics separator of the present invention, and micro- plastics fragment rate of recovery is high, and flotation fluid is Ke Xunhuanliyong, practical and at low cost, can be widely applied to the enrichment isolation of the micro- plastics of environment.
Description
Technical field
The present invention relates to micropollutants technical field of environmental detection, more specifically to a kind of floating and enriching of micro- plastics
Device and its screening technique.
Background technique
Micro- plastics (< 5mm) are as a kind of novel pollutant, since its particle is small, quantity is more, distribution is wide and is easy to by water
Raw biology is ingested, and can release poisonous and harmful substance, such as bisphenol-A, phthalate etc. in water environment, micro- plastics because
Large specific surface area, the easily persistence organic pollutants such as absorption poisonous and harmful substance, such as Polychlorinated biphenyls, polycyclic aromatic hydrocarbon, micro- plastics
Organic contamination sphere is formed with these contaminants, can finally endanger human health by food chain.
Micro- plastics in environment are measured, the enrichment and screening that carry out sample are first had to.In conjunction with literature survey and reality
Border research conditions are it can be found that currently there are still following problems in the micro- plastic monitoring of water environment: first is that sampling, method for separating lack
Weary specification and standard, it is random larger.Second is that flotation, separation and measurement method inefficiency, are unable to satisfy a wide range of, large sample
The investigation and routine monitoring of amount need to reinforce efficient, convenient, cheap, safe technical method research and development.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of floating and enrichings of micro- plastics in recycled water to set
Standby and its screening technique, using this device and method can multiple batches of progress in the lab, realize the efficiently concentrating of micro- plastics.
The purpose of the present invention is achieved by following technical proposals.
The floating and enriching screening plant of micro- plastics of the invention, including flotation fluid liquid storage device and separating pipe, described is floating
It selects by being equipped with the immersion glass pipet connection of outflow valve between liquid liquid storage device and separating pipe, air driven pump goes out
Mouth is connected with the import of tracheae, the mixed solution setting in the outlet alignment flotation fluid liquid storage device of the tracheae, described
Air release valve is installed, the outlet of an aeration pump is equipped with the aeration of air valve with one on the roof of flotation fluid liquid storage device
Pipe is connected, and the aeration head of the aeration tube insertion separating pipe and separating pipe is mounted on bottom in separating pipe, a scum pipe
One end with separate bottom of the tube connection, residual cake valve is installed on the scum pipe, in the upper portion side wall of the separating pipe
On be provided with overflow port, the overflow port be connected to one end of spherical trap and the other end of the spherical trap with
The funnel of Suction filtration device is oppositely arranged.
The floating and enriching screening technique of micro- plastics of the invention, the following steps are included:
Step 1: in saturation NaI or ZnCl2The rhamnolipid as biosurfactant is added in solution, so that mixed
The concentration for closing rhamnolipid in solution is 0.03mmolL-1, removal impurity then is filtered to mixed solution, then will be filtered
Mixed solution injects at separating pipe to tube body volume 1/2, and mixed solution is injected in flotation fluid liquid storage device and is stored up to apart from flotation fluid
At liquid device top surface 1/3；
Step 2: the plastic flakes for crossing 0.5mm sieve are transferred in separating pipe with clean metallic spatula, then first start
Aeration pump opens air valve again, and the bubble generated by the aeration head of aeration tube is in separating pipe bottom purge mixed solution, agitation
The impurity carried secretly in plastic flakes and plastic flakes first closes air valve, is then shut off aeration pump sufficiently after agitation, to be separated
Mixed solution standing in pipe reaches after solid-liquid is sufficiently separated, and obtains clear supernatant；
Step 3: starting air driven pump, pressurizes to the mixed solution in flotation fluid liquid storage device, passes through immersion glass pipet
Solution is slowly pressed into separating pipe, supernatant liquid level is increased to overflow at the overfall of separating pipe in separating pipe, in overflow
Impurity is trapped in spherical trap, and overflowing liquid takes away the plastics floatingly selected, and is collected in the funnel of Suction filtration device；When stopping
When only collecting the supernatant of spilling, the outflow valve being mounted on immersion glass pipet is closed, first to prevent solution from flowing back into
In flotation fluid liquid storage device, the air release valve being mounted on flotation fluid liquid storage device roof is opened, rapidly then to balance flotation fluid
The internal pressure of liquid storage device；
Step 4: carry out vacuum filter to the saline solution containing plastic flakes is collected in Suction filtration device, then incited somebody to action
Flotation fluid after filter is transferred in flotation fluid liquid storage device and reuses, then broken with the plastics retained in distilled water flushing Suction filtration device
Piece several times, to remove salt residue, collects filtered filter membrane, filter membrane is remained in glass dish, be placed under microscope and see
Examine micro- plastics.
The invention has the benefit that (1) flotation fluid is by NaI and ZnCl2Solution replaces NaCl solution, and usual micro- plastics are close
Degree is generally in 0.8-1.4gcm-3, and sediment density is usually 2.65gcm-3, it is saturated NaCl solution, density is
1.2g·cm-3, high polymer cannot be made all to be detached from deposit, will lead to analysis in the micro- plastics of the high density such as separation polyvinyl chloride
As a result serious less than normal.It is saturated NaI and ZnCl2The density of solution is bigger, respectively 1.6-1.8gcm-3With 1.5-1.7g
cm-3, the extraction efficiency to high-density plastic's component can be improved, therefore use NaI or ZnCl2Solution, which impregnate to sample, to be divided
From.(2) in floatation process add low dosage biosurfactant --- rhamnolipid can obviously inhibit bubble deformation,
It reduces the terminal rate of bubble and stablizes its track.Rhamnolipid can promote the generation of microbubble, to increase bubble surface
Product, increases the contact probability of bubble and plastic grain, is conducive to the fluid dynamics environment for improving flotation.(3) FLOTATION SEPARATION
Device is based on density separation principle and extracts micro- plastic grain, and operation cleaning is simple and easy, and sample requirements are few, and micro- plastic grain returns
High income, flotation fluid is Ke Xunhuanliyong, practical and at low cost, can be widely applied to the detection research of micro- plastics in environment
In.
Detailed description of the invention
Fig. 1 is the floating and enriching schematic device of micro- plastics of the invention.
Specific embodiment
Below by specific embodiment, further description of the technical solution of the present invention.
Basic principle of the invention is that bubble adhesion properties on hydrophilic and hydrophobic material can be changed based on surfactant
Difference, highdensity flotation solution can improve to the micro- plastics separating effect of high density.
The floating and enriching screening plant of micro- plastics of the invention, including flotation fluid liquid storage device 4 and separating pipe 7, it is described
By being equipped with the immersion glass pipet connection of outflow valve 11 between flotation fluid liquid storage device 4 and separating pipe 7, one pneumatic
The outlet of pump 2 is connected with the import of tracheae, the mixed solution setting in the outlet alignment flotation fluid liquid storage device 4 of the tracheae,
Air release valve 3 is installed on the roof of the flotation fluid liquid storage device 4.The outlet of one aeration pump 1 is equipped with one
The aeration tube of air valve 8 is connected, and the aeration head 10 of the aeration tube insertion separating pipe 7 and separating pipe 7 is mounted on separating pipe 7
Interior bottom.One end of a piece scum pipe is connected to 7 bottom of separating pipe, is arranged after the end of the experiment for the grains of sand or fine and close impurity particle
Out.Residual cake valve 9 is installed on the scum pipe.
Overflow port 5, the overflow port 5 and the one of spherical trap 6 are provided in the upper portion side wall of the separating pipe 7
End is connected to and the other end of spherical trap 6 and the funnel of Suction filtration device 12 are oppositely arranged.
Preferred spherical trap 6 and the angle of horizontal direction are 15 ° -18 °.It can make cause remaining in overflowing liquid in this way
Close granule foreign in stable water flow be detained again by precipitating.
Preferred aeration head is located at separating pipe tube bottom center.In this way bubble and plastics can be increased with uniform aeration
The contact probability of grain, improves the fluid dynamics environment of flotation.
The floating and enriching screening technique of the micro- plastics of the present invention, comprising the following steps:
Step 1: in saturation NaI or ZnCl2The rhamnolipid as biosurfactant is added in solution, so that mixed
The concentration for closing rhamnolipid in solution is 0.03mmolL-1, removal impurity then is filtered to mixed solution, then will be filtered
Mixed solution injects at separating pipe 7 to tube body volume 1/2, and mixed solution is injected in flotation fluid liquid storage device 4 to apart from flotation fluid
At 4 top surface 1/3 of liquid storage device.
Step 2: the plastic flakes for crossing 0.5mm sieve are transferred in separating pipe 7 with clean metallic spatula.Then it first opens
Pneumatic aeration pump 1 opens air valve 8 again, and the bubble generated by the aeration head 10 of aeration tube mixes molten in 7 bottom purge of separating pipe
Liquid stirs the impurity carried secretly in plastic flakes and plastic flakes.Sufficiently after agitation, air valve 8 is first closed, aeration pump is then shut off
1.Mixed solution standing in pipe 7 to be separated reaches after solid-liquid is sufficiently separated, and obtains clear supernatant.
Step 3: starting air driven pump 2, pressurizes to the mixed solution in flotation fluid liquid storage device 4, passes through immersion glass liquid relief
Solution is slowly pressed into separating pipe 7 by pipe.Supernatant liquid level is increased to 5 spilling at the overfall of separating pipe 7 in separating pipe 7, overflows
Impurity in stream is trapped in spherical trap 6, and overflowing liquid takes away the plastics floatingly selected, and is collected in the leakage of Suction filtration device 12
In bucket.When stopping collecting the supernatant overflowed, the outflow valve 11 being mounted on immersion glass pipet is closed, first to prevent
Solution flows back into flotation fluid liquid storage device 4.Then the air release valve 3 being mounted on 4 roof of flotation fluid liquid storage device is opened rapidly,
To balance the internal pressure of flotation fluid liquid storage device.
Step 4: carrying out vacuum filter to the saline solution containing plastic flakes collected in Suction filtration device 12, then will
Filtered flotation fluid is transferred in flotation fluid liquid storage device 4 and reuses.Again with retaining in distilled water flushing Suction filtration device 12
Plastic flakes several times, to remove salt residue.Filtered filter membrane (aperture can be 0.45 μm) is collected, filter membrane is remained in
In glass dish, it is placed in the micro- plastics of microscopically observation.
It preferably, will if the content of organic matter that adheres to of the plastic flakes on the filtered filter membrane of Suction filtration device 12 is higher
Plastic flakes on filter membrane and filter membrane are put into togerther digestion tube, and digestive reagent is added and clears up at 70 DEG C, until resolution liquid becomes
Clarification.Then ultrapure water is added in digestion tube, then the resolution liquid that ultrapure water is added is injected into 12 vacuum filter of Suction filtration device,
Finally with the plastic flakes retained in distilled water flushing Suction filtration device, filtered filter membrane (0.45 μm of aperture) is collected, is remained in
In glass dish, it is placed in microscopically observation plastic flakes.The H that the digestive reagent is 30% by mass percent2O2And quality
The HNO that percentage is 65%3Composition, the H2O2And HNO3Volume ratio be 1:3.
The present invention is directed to environmental water sample, by optimizing micro- flotation of Plastics solution, adds surfactant, it is close to improve micro- plastics
Spend separation process, can in the analysis water of efficiently and accurately micro- plastics status of accumulating nutrient, the rate of recovery of micro- plastics can reach in water sample
97%, micro- plastics of recycling are used for the subsequent research to micro- plastics shape characteristic and its surface attachment.
It is demonstrated experimentally that successfully obtaining micro- plastics in sample with the device, demonstrating the applicability of the separation method.
Using the device and flotation separation method, find to exist in environmental water sample particulate species (polyethylene), foaming kind (polystyrene),
Fiber-like (low density polyethylene (LDPE)), fragment class (polyethylene or polypropylene) and film class (polypropylene) micro- plastics.
The spatially relative terms such as "upper", "lower", "left", "right" have been used in embodiment for ease of explanation, have been used for
Relationship of the elements or features relative to another elements or features shown in explanatory diagram.It should be understood that in addition to figure
Shown in except orientation, spatial terminology is intended to include the different direction of device in use or operation.For example, if in figure
Device be squeezed, the element for being stated as being located at other elements or feature "lower" will be located into other elements or feature "upper".
Therefore, exemplary term "lower" may include both upper and lower orientation.Device, which can be positioned in other ways, (to be rotated by 90 ° or position
In other orientation), it can be interpreted accordingly used herein of the opposite explanation in space.
Moreover, the relational terms of such as " first " and " second " or the like are used merely to one with another with identical
The component of title distinguishes, without necessarily requiring or implying between these components there are any this actual relationship or
Sequentially.
It describes the invention in detail, but content is only the preferred embodiment of the present invention, cannot be recognized above
For for limiting practical range of the invention.Any changes and modifications in accordance with the scope of the present application should all still return
Belong within patent covering scope of the invention.
Claims (5)
1. the floating and enriching screening plant of micro- plastics, it is characterised in that: including flotation fluid liquid storage device and separating pipe, described is floating
It selects by being equipped with the immersion glass pipet connection of outflow valve between liquid liquid storage device and separating pipe, air driven pump goes out
Mouth is connected with the import of tracheae, the mixed solution setting in the outlet alignment flotation fluid liquid storage device of the tracheae, described
Air release valve is installed, the outlet of an aeration pump is equipped with the aeration of air valve with one on the roof of flotation fluid liquid storage device
Pipe is connected, and the aeration head of the aeration tube insertion separating pipe and separating pipe is mounted on bottom in separating pipe, a scum pipe
One end with separate bottom of the tube connection, residual cake valve is installed on the scum pipe, in the upper portion side wall of the separating pipe
On be provided with overflow port, the overflow port be connected to one end of spherical trap and the other end of the spherical trap with
The funnel of Suction filtration device is oppositely arranged.
2. the floating and enriching screening plant of micro- plastics according to claim 1, it is characterised in that: the spherical trap
Angle with horizontal direction is 15 ° -18 °.
3. the floating and enriching screening plant of micro- plastics according to claim 1 or 2, it is characterised in that: the aeration
Head is located at separating pipe tube bottom center.
4. using the floating and enriching screening technique of one of claim 1-3 micro- plastics of device, it is characterised in that including following step
It is rapid:
Step 1: in saturation NaI or ZnCl2The rhamnolipid as biosurfactant is added in solution, so that mixed solution
The concentration of middle rhamnolipid is 0.03mmolL-1, removal impurity then is filtered to mixed solution, then filtered mixing is molten
Liquid injects at separating pipe to tube body volume 1/2, and mixed solution is injected in flotation fluid liquid storage device to apart from flotation fluid liquid storage device top
At face 1/3；
Step 2: the plastic flakes for crossing 0.5mm sieve are transferred in separating pipe with clean metallic spatula, then first starting is aerated
Pump opens air valve again, and the bubble generated by the aeration head of aeration tube stirs plastics in separating pipe bottom purge mixed solution
The impurity carried secretly in fragment and plastic flakes first closes air valve, is then shut off aeration pump sufficiently after agitation, in pipe to be separated
Mixed solution standing reach after solid-liquid is sufficiently separated, obtain clear supernatant；
Step 3: starting air driven pump, pressurizes to the mixed solution in flotation fluid liquid storage device, it will be molten by immersion glass pipet
Liquid is slowly pressed into separating pipe, and supernatant liquid level is increased to overflow at the overfall of separating pipe in separating pipe, the impurity in overflow
It is trapped in spherical trap, overflowing liquid takes away the plastics floatingly selected, and is collected in the funnel of Suction filtration device；When stopping is received
When collecting the supernatant overflowed, the outflow valve being mounted on immersion glass pipet is closed, first to prevent solution from flowing back into flotation
In liquid liquid storage device, the air release valve being mounted on flotation fluid liquid storage device roof is opened, rapidly then to balance flotation fluid liquid storage
The internal pressure of device；
Step 4: vacuum filter is carried out to the saline solution containing plastic flakes collected in Suction filtration device, after then filtering
Flotation fluid be transferred in flotation fluid liquid storage device and reuse, then it is several with the plastic flakes retained in distilled water flushing Suction filtration device
It is secondary, to remove salt residue, filtered filter membrane is collected, filter membrane is remained in glass dish, it is micro- to be placed in microscopically observation
Plastics.
5. according to the floating and enriching screening technique of the micro- plastics of claim 4, it is characterised in that: if the filtered filter membrane of Suction filtration device
On plastic flakes adherency the content of organic matter it is higher, then the plastic flakes on filter membrane and filter membrane are put into togerther digestion tube, added
Enter digestive reagent to clear up at 70 DEG C, until resolution liquid becomes clarification, ultrapure water is then added in digestion tube, then super by being added
The resolution liquid of pure water injects Suction filtration device vacuum filter, finally with the plastic flakes retained in distilled water flushing Suction filtration device,
Filtered filter membrane is collected, is remained in glass dish, is placed in microscopically observation plastic flakes, the digestive reagent is by quality
The H that percentage is 30%2O2The HNO for being 65% with mass percent3Composition, the H2O2And HNO3Volume ratio be 1:3.
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| CN201811321283.4A CN109655321A (en) | 2018-11-07 | 2018-11-07 | The floating and enriching device and its screening technique of micro- plastics |
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| CN110286004A (en) * | 2019-07-11 | 2019-09-27 | 叶建锋 | The acquisition method and device of a kind of micro- plastics sedimentation of atmosphere for different height |
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| CN110369117A (en) * | 2019-08-14 | 2019-10-25 | 中国环境科学研究院 | A kind of device and method efficiently separating the micro- plastics of flotation |
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Application publication date: 20190419 |