CN109877150A - A kind of device and method based on the circulating separation micro- plastics of soil of sodium bromide solution - Google Patents

A kind of device and method based on the circulating separation micro- plastics of soil of sodium bromide solution Download PDF

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Publication number
CN109877150A
CN109877150A CN201910028203.4A CN201910028203A CN109877150A CN 109877150 A CN109877150 A CN 109877150A CN 201910028203 A CN201910028203 A CN 201910028203A CN 109877150 A CN109877150 A CN 109877150A
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plastics
micro
soil
sodium bromide
separator
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何德富
刘梦婷
陆诗博
宋杨
曹承进
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East China Normal University
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East China Normal University
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Abstract

The invention discloses a kind of devices based on the circulating separation micro- plastics of soil of sodium bromide solution, comprising: separation system, vacuum filtration system and solution recovery system;Wherein, the separation system includes: separator, aeration plate, pallet, adjustable aeration pump;The vacuum filtration system includes: bottle,suction, vacuum filtration pump, sand core filter;The solution recovery system includes: separatory funnel, circulating pump.The invention also discloses a kind of methods based on the circulating separation micro- plastics of soil of sodium bromide solution.The present invention selects separation agent of the saturation sodium bromide as the micro- plastics of soil; in conjunction with aeration process; micro- plastics are made to float on soil mixed liquor upper layer; after solution left standstill layering, micro- plastics are overflowed from container hole using the power that aeration and solution add, micro- plastics are collected by Vacuum filtration device; sodium bromide solution is recycled by recovery system; cost is greatlyd save, and realizes the low emission of sodium bromide, is conducive to protect environment.

Description

A kind of device and method based on the circulating separation micro- plastics of soil of sodium bromide solution
Technical field
The invention belongs to separation technology fields, are related to a kind of dress based on the circulating separation micro- plastics of soil of sodium bromide solution It sets and method.
Background technique
With plastics mass production and use, micro- plastic pollution that fragmentation is formed is had recently received great interest.Micro- modeling Material is small plastics (Thompson R C, Russell A E.Lost at sea:where is all that size is less than 5mm The plastic? Science, 2004,304 (5672): 838), including the different shapes such as fragment, fiber, particle and film, again It is divided into the multiple types such as polyethylene, polypropylene, polyvinyl chloride.Since a large amount of plastics are discarded into surface soil environment, how from soil This plastics slightly is separated in earth medium, is a urgent problem to be solved.
Separation for plastics micro- in complex dielectrics, conventional method are based primarily upon Density Separation principle, rise by gas Or aqueous agitation, micro- plastics are isolated from sample, but the rate of recovery is low, complex steps, time-consuming.With simple flotation point The micro- plastics of semi-automatic separation may be implemented in appearance from device, and the rate of recovery is improved, but that there are still manual interventions is more, The problems such as time-consuming.Zhang Haibo et al. applies for having invented a kind of continuous flowing separating flotation device and method of microparticle plastics (number of patent application 201510227085.1) realizes the continuous flowing flotation of solid sample.But the device is made by air Carry out separating and filtering for medium, it is not easy to so that micro- plastics is floated completely, thus recovery efficiency is not high.Zhang Kai et al. has invented a kind of micro- Rear suspension is sufficiently stirred using sample is filled inside cylindrical body in plastic selector (Authorization Notice No. CN206106152U) It stands, obtains micro- plastics of separation and Extraction with membrane filtration non-precipitating layer part.But solution and micro- plastics are separated in practical operation The suspension of formation is easily attached to separation column wall, reduces separative efficiency.The orchid of in August, 2018 sheath or bow case etc. has applied for that one kind is based on ZnCl2Solution fractionation separates the device (application number 201810948733.6) of micro- plastics and cellulose crystallite in soil, but the party Method process is cumbersome, takes a long time.
Previous micro- plastics separation method mostly uses greatly the NaCl solution of low-density, although cheap and environmental sound, But the micro- plastics of high density (such as polyvinyl chloride) cannot efficiently separate, and cause a variety of micro- plastics recovery rates very low;Individual researchers adopt Micro- plastics are separated with higher density solutions such as NaI, but it is expensive, and separating liquid flows into environment, has ecological environment harm.
Existing to separate micro- plastic processes and device, by manual operation, complex steps are taken a long time;In addition, micro- plastics Usually it is adhered to walls of beaker, it is difficult to rinse completely, cause effective rate of recovery low.
Summary of the invention
In order to overcome the above-mentioned defects in the prior art, the invention proposes one kind to be based on the circulating separation of sodium bromide solution The device and method of the micro- plastics of soil.Present invention seek to address that the reagent consumption in the micro- plastic separation process of soil is big, time-consuming Difficult problem is separated with the micro- plastics of high density.
In the present invention, micro- plastics include polyamide (PA), polypropylene (PP), polyethylene (PE), poly terephthalic acid Glycol ester (PET), polyformaldehyde (POM), polyvinyl chloride (PVC), polycarbonate (PC), acronitrile-butadiene-styrene (ABS), One or more micro- plastics such as polymethyl methacrylate (PMMA), polystyrene (PS).
The invention proposes a kind of devices based on the circulating separation micro- plastics of soil of sodium bromide solution comprising: separation System, vacuum filtration system and solution recovery system;Wherein, the separation system includes: separator, aeration plate, pallet, aeration Pump;The vacuum filtration system includes: bottle,suction, vacuum filtration pump, sand core filter;The solution recovery system includes: point Liquid funnel, circulating pump;
Wherein, the separatory funnel lower end is suspended in the separator.
The aeration plate is arranged in the separator bottom;The aeration plate is connect with the aeration pump.
The separator outer wall is arranged the pallet and forms the cavity for accommodating and collecting spillage.
The pallet, sand core filter, bottle,suction, circulating pump, separatory funnel pass sequentially through rubber tube connection and realize circulation;
The bottle,suction is connected to vacuum filtration pump.
Wherein, separator place suitable for reading is provided with through-hole, the speed of liquid outflow can be alleviated, while stopping big modeling The spilling of material;Preferably, separator place suitable for reading is provided with 2 exhausting holes.
The diameter of the through-hole is 5mm;
Spacing between the through-hole and through-hole is 2-3mm;It preferably, is 2mm.
Wherein, the pallet is hollow, and left and right ends bottom has difference in height, and the gradient that the difference in height is formed is 20-30°;It preferably, is 30 °.
Liquid outlet is arranged in the pallet lower end, and liquid outlet internal diameter is 5mm, outer diameter 6mm.The convenient liquid overflowed from separator Body directly drains into the filter membrane on piece of sand core filter.
The through-hole of separator of the present invention guarantees that all liquid overflowed from separator drain into the pallet The filter membrane on piece of sand core filter.
The present invention for the pallet diameter control be greater than the separator diameter be 1-2cm;Preferably, it is 1cm.So that spillage uniformly flows out, viscous wall is reduced.
Wherein, the structure of the aeration plate is semielliptical shape, and the size of aeration plate is 80 × 8/4mm of φ, will with rubber tube Aeration plate is connected with aeration pump, and the maximum intensity of aeration pump is 2 × 4.5L/min, and minimum 0, according to light materials in soil sample Amount, adjusts the intensity of aeration pump, if the light materials to float are more, the intensity of aeration pump tunes up therewith.
Wherein, the aeration pump is adjustable aeration pump.
Wherein, filter membrane piece is placed on the sand core filter, the diameter of the filter membrane piece is 47mm, and aperture is 20 μm.
The present invention places the filter membrane piece that aperture is 20 μm on sand core filter, according to the amount of filter membrane on piece trapped substance, more New filter membrane piece.The soil sample less for content of organics, a filter membrane piece;The soil sample more for content of organics, more New 1-2 filter membrane piece.
Wherein, piston-type switch is arranged in the bottle,suction lower end, controls out liquid.
In the present invention, design the advantages of combining chromatographic column and bottle,suction of bottle,suction setting piston-type switch.On the one hand, Sand core filter is matched using the outer grinding port of bottle,suction, has the function that retain micro- plastics in soil.On the other hand, chromatography is utilized Switch designs in the form of piston in column, the width of chromatographic column is widened, and expands capacity, and liquid can flow out from Qi Xiakou and facilitate receipts Collection.
Further, device of the present invention further include: lifting platform and iron stand.
The separator is fixed on the iron stand by the lifting platform;The separatory funnel is fixed on the brandreth On platform.
The power that liquid in separator of the present invention is put into and is aerated by liquid circulation can be overflowed from through-hole, The fixed pallet with difference in height outside separator is in order to drain into the liquid overflowed directly on filter membrane, when saving separation Between, shorten process, reduces viscous wall.
Separator housing fixed tray form is arranged in separation system in the present invention, and pallet has difference in height, Ke Yishi Solution constant flow in existing pallet had not only guaranteed that solution flowed into filter membrane, but also has reduced wall sticking phenomenon;Under vacuum filtration system uses Piston type is held to be discharged bottle,suction, upper set sand core filter is opened always during suction filtration, realizes the effect recycled when filtering Fruit;Vacuum filtration system is different from traditional bottle,suction, and while micro- plastics are trapped, the liquid in bottle,suction can be flowed into In circulating pump, necessary condition is provided for the recycling of solution, since the piston of bottle,suction is opened, liquid can be flowed into phase therewith The rubber tube of connection, rubber tube are connect with circulating pump again, and liquid is pumped into separatory funnel by circulating pump, realize circulate operation.
In addition, compared with prior art, the invention improves the structure of bottle,suction, bottle,suction is connect with circulating pump, is realized Automation filters and cyclic process, reduces process, saves reagent;It is applied widely, it is suitble to a variety of different types of micro- modelings of separation Material;Apparatus integration also can be used alone, convenient and efficient, improve the recall rate of micro- plastics, realize the company of micro- plastics in soil Continuous flotation, the recycling of separation agent.
Based on apparatus above, the present invention also provides a kind of sides based on the circulating separation micro- plastics of soil of sodium bromide solution Method:
(1) saturation sodium bromide solution and soil are put into togerther in separator, after being stirred, are aerated and are stood;
(2) supernatant liquid after standing to step (1) is persistently aerated, while addition saturation sodium bromide is molten in separatory funnel Liquid opens the valve of separatory funnel, and liquid is allowed to flow into separator;And then overflowed from separator through-hole, open simultaneously vacuum Suction filter pump, circulating pump, the separation of the achievable micro- plastics of soil.
In step (1), the time of the aeration is 20-30min;It preferably, is 30min.
In step (1), the time of the standing is 1-2h;It preferably, is 2h.
In step (1), the mass ratio of the saturation sodium bromide solution and soil is (2-3): 1;It preferably, is 2:1.
In step (1), the soil is preferably the soil dried.
In step (2), the vacuum filtration pressure is 0-0.08MPa;It preferably, is 0.04MPa.
In step (2), the pump flow range is 19-100ml/min;It preferably, is 80ml/min.
Further include pre-treatment step before step of the present invention (1): grinding soil, and 5mm sieve is crossed, it removes in soil Bulky grain.
Reagent currently used for separating micro- plastics is mainly sodium chloride, is also had using zinc chloride, calcium chloride and sodium iodide etc. 's.Essentially consist in: sodium chloride and calcium chloride are cheap, but density is lower, can not isolate the micro- plastics of high density;Zinc chloride It is at high price although high with sodium iodide density, and have certain toxicity.Therefore, the present invention selects moderate cost, density high Sodium bromide can efficiently separate all kinds of micro- plastics, and environmental hazard is few.
In a specific embodiment, the method based on the circulating separation micro- plastics of soil of sodium bromide solution is specific The following steps are included:
Pretreatment process: firstly, preparing saturation sodium bromide solution;Weigh drying soil 50g.Then, by configured bromination Sodium solution pours into separator, places aeration plate, load weighted soil sample is added to the container, and starts to be aerated 30min, aeration terminates Afterwards, 1-2h is stood.
Treatment process: the solution containing soil sample after standing will appear lamination, carry out duration aeration to upper liquid, simultaneously Add a small amount of sodium bromide solution;Due to the power for adding and being aerated of solution, solution is overflowed from through-hole, flows into vacuum filtration system In, micro- plastics are trapped on filter paper, and filtered sodium bromide solution flows into bottle,suction;By the power of circulating pump, by bromine Change sodium solution to extract out from bottle,suction, re-enter into the solution containing soil sample;The process is continuously circulated 30min, it is therefore an objective to make Micro- plastics are totally separated and are collected in soil.
The present invention carries out separating the technology that the micro- plastics of soil need to overcome using saturation sodium bromide solution and described device to be stranded It is difficult to include: with difficult point
1, during filtering, it may be accumulated due to soil sample on filter membrane and micro- plastics, suction filtration is caused to slow, it should be noted that And filter membrane piece is replaced in time.
2, in cyclic process, the pressure according to suction filter pump is needed, adjusts the flow velocity of circulating pump, is just able to achieve and is followed when filtering The process of ring.
Mainly by aerating system, system and solution recovery system group is filtered by vacuum in the micro- plastic selector of soil of the invention At.The innovative point of the device includes:
1) separator place suitable for reading devise two rows of diameters be 5mm through-hole, above an exhausting hole distance separation device mouth upper limb 1cm, gap is 2mm between each through-hole, and through-hole surfaces are smooth, can be with continuous punching by solution circulating and aeration process Through-hole is washed, is not susceptible to block;It is directly overflowed compared to mouth from container, which overflows uniformly, and speed is gentle.
2) one pallet with difference in height of separator housing, the gradient are 30 °, and surface is smooth, is conducive to the liquid overflowed Body, which is taken advantage of a situation, continues into suction filtration system, reduces micro- plastics and glues wall, improves the rate of recovery.
3) aerating system can not only be such that the soil liquid sufficiently stirs, and will not block the through-hole on separator, also be micro- Plastics, which overflow, provides power, is improved efficiency by continuously stirring separation.
4) present invention innovative design separating liquid recovery system in micro- plastic selector realizes the weight of separation solution It is multiple to utilize, it reduces costs, and realize environmentally protective.
Generally, the technical solution of this invention can reach simultaneously separation the micro- plastics of soil low cost, high efficiency and Multi-cycle separation purpose.
The present invention selects separation agent of the saturation sodium bromide as the micro- plastics of soil, in conjunction with aeration process, keeps micro- plastics floating In soil mixed liquor upper layer, after solution left standstill layering, make micro- plastics from container hole using the power that aeration and solution add It overflows, micro- plastics is collected by Vacuum filtration device, sodium bromide solution is recycled by recovery system.
Beneficial effects of the present invention further include: the utilization of the present apparatus can make polyamide (PA), polypropylene (PP), polyethylene (PE), polyethylene terephthalate (PET), polyformaldehyde (POM), polyvinyl chloride (PVC), polycarbonate (PC), acrylonitrile Butadiene styrene (ABS), polymethyl methacrylate (PMMA) and a variety of micro- plastics of polystyrene (PS) are efficient in the soil Rate separation, wherein up to 96.7% or more, (wherein PA, PC, PE, PS recall rate are 100%, PP to the recall rate of the micro- plastics of low-density Recall rate is 98.3%, ABS, 96.7%) PMMA recall rate is;The separation rate of the micro- plastics of high density be 90%-100% (wherein PET recall rate is that 100%, POM recall rate is 98.3%, PVC recall rate for 90%).Secondly, disengaging time can be saved, by Artificial separation method is reduced to 2-3h for 24 hours, improves work efficiency.Furthermore since the recycling of NaBr separation solution repeats benefit With, greatly save cost, and realize the low emission of NaBr, be conducive to protect environment.
Detailed description of the invention
Fig. 1 is the micro- plastic selector schematic diagram of soil.
Specific embodiment
In conjunction with following specific embodiments and attached drawing, the present invention is described in further detail.Implement process of the invention, Condition, experimental method etc. are among the general principles and common general knowledge in the art, this hair in addition to what is specifically mentioned below It is bright that there are no special restrictions to content.
Fig. 1: 1- separatory funnel, 2- separator, 3- aeration plate, 4- lifting platform, 5- iron stand, 6- circulating pump, 7- bottle,suction, 8- vacuum filtration pump, 9- sand core filter, 10- pallet, the adjustable aeration pump of 11-, remaining is rubber tube.
Embodiment 1
It is to detect the separative efficiency of the micro- plastics of PA, PP, PE, PET, POM, PVC, PC, ABS, PMMA and PS in the soil Example
Detailed process:
1. weighing 50g soil sample, (soil sample is the normal soil sample acquired from campus, does not do micro- plastics removal processing, but implement Micro- plastics of example 1-3 addition are micro- plastics by dyeing processing).
2. the one species for selecting 20 sizes in 1-3mm pass through the micro- plastics of graininess of Nile red dye marker (such as PP), it is uniformly blended into soil sample
3. preparing 200ml is saturated sodium bromide solution.
4. pouring into 100ml saturation sodium bromide solution in 2- separator, aerator is opened, then pour into the soil mixed Sample.
5. 3- aeration plate connects the adjustable aeration pump of 11-, it is aerated 30min, is then allowed to stand 2h.
6. separator is put into the micro- plastic selector of soil, the filter in 20 μm of aperture is placed on 9- sand core filter Film.
7. being persistently aerated after standing to supernatant liquid, while addition 50ml saturation sodium bromide is molten in 1- separatory funnel Liquid opens valve, and liquid is allowed to flow into separator.
8. solution is constantly spilled over to 10- pallet from the gap 5mm and opens simultaneously 8- vacuum filtration pump, start to filter.
9. opening 6- circulating pump, sodium bromide solution in 7- bottle,suction is pumped into again in 1- separatory funnel.
10. repeat it is above-mentioned 7. -9. step, 30min.
With sodium bromide solution repeated flushing 10- pallet 3 times.
Micro- plastics number on filter membrane is counted, the rate of recovery is counted.
After experiment, by vacuum filtration, circulation pump recycles whole sodium bromide solutions, storage.
Experiment is parallel to repeat 3 groups.
The micro- plastics of ten seed types carry out above-mentioned experimentation respectively, the results showed that PA, PP, PE, PC, PS, ABS, PMMA are micro- The rate of recovery of plastics is up to 96.7%, and plastics PET micro- for high density, the rate of recovery of POM, PVC also reaches 90%-100%.
Embodiment 2
By taking PE as an example, selecting partial size is respectively 100-500 μm, and 500-1000 μm, 1000-3000 μm of the micro- modeling of PE graininess Material, is tested respectively, and for detailed process referring to embodiment 1, the rate of recovery of the micro- plastics of the PE of 3 kinds of partial sizes is respectively 83%, 95%, 100%.
Embodiment 3
By taking PE as an example, film-form, threadiness, the recycling of the micro- plastics of graininess PE (500-1000 μm) in the soil are studied Rate, detailed process respectively reach 80%, 83%, 95% referring to embodiment 1, the rate of recovery of the micro- plastics of the PE of 3 kinds of shapes.
Embodiment 4
By taking field acquisition soil sample as an example, drying soil sample 100g is weighed, prepares sodium bromide solution 300ml, next operation step Suddenly identical as the embodiment of the present invention 1, it detects that the form of micro- plastics has 3 kinds, is threadiness, film-form and graininess respectively;It is micro- Plastics kind has PP, PE, PET and PA, detects 38 micro- plastics (having a size of 57-4617 μm).
Overall effect:
The utilization of the micro- plastic selector of soil through the invention, can be all kinds of to soil micro- within the short period (~2h) Plastics are efficiently separated, and realize that separating liquid recycles, and reach effects of energy conservation and environmental protection.
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with appended claims be protect Protect range.

Claims (10)

1. a kind of device based on the circulating separation micro- plastics of soil of sodium bromide solution, which is characterized in that described device includes: point From system, vacuum filtration system and solution recovery system;Wherein,
The separation system includes: separator (2), aeration plate (3), pallet (10), aeration pump (11);
The vacuum filtration system includes: bottle,suction (7), vacuum filtration pump (8), sand core filter (9);
The solution recovery system includes: separatory funnel (1), circulating pump (6);
Separatory funnel (1) lower end is located in the separator (2);
The aeration plate (3) is arranged in separator (2) bottom, and the aeration plate (3) connect with the aeration pump (11);
The separator (2) and the pallet (10) form an entirety, accommodate and collect liquid;The pallet (10), sand core Filter (9), bottle,suction (7), circulating pump (6), separatory funnel (1) pass sequentially through rubber tube connection and realize circulation;
The bottle,suction (7) pumps (8) with the vacuum filtration and is connected to;
The part that the separator (2) is located in the pallet (10) is provided with through-hole.
2. device as described in claim 1, which is characterized in that described device further comprises: lifting platform (4), iron stand (5);The separatory funnel (1) is fixed on the iron stand (5);The separator (2) is fixed on by the lifting platform (4) On the iron stand (5).
3. device as described in claim 1, which is characterized in that the diameter of the through-hole is 5mm;The through-hole spacing is 2- 3mm。
4. device as described in claim 1, which is characterized in that the pallet (10) is provided with the gradient, and the gradient size is 20-30°。
5. device as described in claim 1, which is characterized in that the structure of the aeration plate (3) is semielliptical shape, the aeration The size of disk is 80 × 8/4mm of φ;The intensity of the aeration pump (11) is 0-2 × 4.5L/min.
6. device as described in claim 1, which is characterized in that the liquid outlet internal diameter of the pallet (10) is 5mm, and outer diameter is 6mm。
7. device as described in claim 1, which is characterized in that piston-type switch is arranged in bottle,suction (7) lower end, controls out Liquid.
8. device as described in claim 1, which is characterized in that be provided with filter membrane piece on the sand core filter (9).
9. a kind of method based on the circulating separation micro- plastics of soil of sodium bromide solution, which is characterized in that the method are as follows: will satisfy Be put into togerther in separator with sodium bromide solution and soil, after being stirred, be aerated and stood, then to aforementioned standing after Supernatant liquid is persistently aerated, while saturation sodium bromide solution being added in separatory funnel, is opened the valve of separatory funnel, is allowed liquid It flows into separator;And then overflowed from separator through-hole, vacuum filtration pump, circulating pump are opened simultaneously, realizes the micro- plastics of soil Separation.
10. the method as claimed in claim 9 based on the circulating separation micro- plastics of soil of sodium bromide solution, which is characterized in that Using described in any item devices of such as claim 1-8.
CN201910028203.4A 2019-01-11 2019-01-11 A kind of device and method based on the circulating separation micro- plastics of soil of sodium bromide solution Pending CN109877150A (en)

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CN113843268B (en) * 2021-09-18 2022-08-05 贵州大学 Separation device and separation method for karst farmland soil micro-plastic

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