CN109228022A - A kind of enriching apparatus and its application method quickly continuously separating micro- plastics - Google Patents
A kind of enriching apparatus and its application method quickly continuously separating micro- plastics Download PDFInfo
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- CN109228022A CN109228022A CN201811183853.8A CN201811183853A CN109228022A CN 109228022 A CN109228022 A CN 109228022A CN 201811183853 A CN201811183853 A CN 201811183853A CN 109228022 A CN109228022 A CN 109228022A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
- B29B17/02—Separating plastics from other materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
- B29B17/02—Separating plastics from other materials
- B29B2017/0213—Specific separating techniques
- B29B2017/0217—Mechanical separating techniques; devices therefor
- B29B2017/0224—Screens, sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
- B29B17/02—Separating plastics from other materials
- B29B2017/0213—Specific separating techniques
- B29B2017/0217—Mechanical separating techniques; devices therefor
- B29B2017/0248—Froth flotation, i.e. wherein gas bubbles are attached to suspended particles in an aerated liquid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Mechanical Engineering (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A kind of enriching apparatus and its application method quickly continuously separating micro- plastics.The device includes flotation fluid cyclic part and sample separation and concentration part;The flotation fluid cyclic part includes peristaltic pump, liquid storage bottle, flowmeter, filters cylinder, vacuum pump and conduit, sample separation and concentration part includes ultrasonic generator, sample bottle, flotation pipe, stirring rod and multi-stage screening disk, filters cylinder and is placed in ultrasonic generator;Sample bottle, which is placed in, to be filtered in cylinder, and flotation pipe is assembled on sample bottle, if finally dry sieving disk is nested on the outside of flotation pipe;Stirring rod is protruded into sample bottle;Cylinder will be filtered to be connected with vacuum pump, the strainer or filter membrane of different-grain diameter are placed in the screening disk.The present invention is designed based on Density Separation principle, and feature is as follows: the flotation fluid recycling between three again reduces economic cost, and do not cause secondary pollution;The setting of multi-stage screening disk can continuously be finely divided micro- plastic grain of different-grain diameter, and separative efficiency is high.
Description
Technical field
The present invention relates to a kind of extraction elements of the micro- plastics of quick separating, and in particular to a kind of quickly continuously to separate micro- plastics
Enriching apparatus and its application method.
Background technique
For the materials such as timber, metal, plastic products are at low cost, and have biggish weight strength, lower
The advantages that pyroconductivity, durability and biologically inert, is applied to every field, for example, using from household supplies to personal hygiene
Product, again from packing business to construction material etc..Enjoy plastic products bring it is huge convenient while, a large amount of plastics
The refuse pollution problem of product also annoyings people.A large amount of plastic products rubbish is discharged into water body environment, especially in sea
Midocean.The plastic products of bulk pass through the effects of light degradation, bioerosion, mechanical degradation in marine environment, are gradually decomposed
At short grained plastics, plastic material fiber, particle and fragment etc. of this size less than 5mm are defined as micro- plastics.Until 20
The pollution problem at century 70 initial stage, little particle plastics is just suggested.
At present in arctic regions, island, continental shelf and deep-sea ocean bottom, or even all detect in salt micro-
The presence of plastics.Since substantial amounts, shape and the diversified micro- plastics of color migrate between different surrounding mediums,
After especially micro- plastics enter ocean, micro- plastics with bigger serface are easy the pollutant in adsorbing seawater, and (persistence has
Machine pollutant and heavy metal ion etc.) and microorganism, become pollutant and microorganism carrier.And micro- plastics of different-grain diameter,
Different toxicological effects can be generated, such as: micro- plastics of Nano grade can carry out into the cell, generating organism with penetrating cell wall
Harm, with the comparable micro- plastics of planktonic organism size, is easily absorbed by marine organisms, and then through food chain between each trophic level
Transmitting, may will affect the entire ecosystem.Therefore, micro- plastics of variable grain are efficiently collected, the micro- plastics of variable grain are evaluated
Harm to environment becomes the matter of utmost importance of the area research, carries out the research policy of micro- plastic pollution control with this.
Current most micro- plastics extraction element is to utilize the density contrast of object and impurity based on Density Separation principle
Different and design device.Such as: the continuous separation and concentration device of Chinese patent (Patent No.: CN 108177273A) micro- plastics,
It is to be mixed into the flotation agent for carrying micro- plastics using gaseous mediums and density fluid, achievees the purpose that the separation of micro- plastics, but not
Micro- plastics of different-grain diameter can be sieved, and can not effective Extraction and enrichment to the micro- plastics being wrapped in sludge.Separately
Outside, Chinese patent (Patent No.: 108202428 A of CN) is a kind of micro- plastics extraction element based on electrostatic technique, although
Micro- plastics in deposit can effectively be extracted, but can not effectively extract short grained micro- plastics and be wrapped in
Micro- plastics in silt and pollutant can not separate micro- plastics of different-grain diameter.Although most micro- plastics point
It can be realized micro- plastics from the automatic continuous separation in deposit from extraction element, but in actual experimentation, often
Often there are micro- plastics and be attached to micro- plastics that vessel surface is not easy to fall and wrapped up being not easy to be extracted, proposes final separation
The micro- plastics result taken is very big in actual difference.
Develop a kind of structure it is simple, can popularity uses, is low in cost, assembling easy to disassemble, maintenance difficulties are low micro- modeling
Expect separation and concentration device, is that micro- plastics study matter of utmost importance in the urgent need to address.The present invention is based on the designs of Density Separation principle
One kind quickly, high-efficiency and continuous separation the micro- plastics of different-grain diameter device.The screening and enrichment of object can be realized according to demand,
Screening efficiency is high, and the recycling of flotation fluid can obviously reduce the dosage of solution, reduces economic cost, and two caused by environment
Secondary pollution is small.
Summary of the invention
The main purpose of the present invention is to provide a kind of separation and concentration device of micro- plastics in deposit, secondary objective exists
In provide it is a kind of using the device separation deposit in micro- plastics application method.
The present invention is designed based on Density Separation principle, and feature is as follows: the recycling between three again of 1. flotation fluids reduces
Economic cost, and do not cause secondary pollution;2. multi-stage screening disk setting can continuously to micro- plastic grain of different-grain diameter into
Row subdivision, separative efficiency are high;The apparatus structure is simple, is easy to split, and is easily installed, carries and safeguards.
Technical scheme is as follows.
A kind of enriching apparatus quickly continuously separating micro- plastics, the recycling of flotation fluid and the micro- plastic grain of different-grain diameter
Continuous separation.Including flotation fluid cyclic part and sample separation and concentration part;The flotation fluid cyclic part include peristaltic pump,
Liquid storage bottle, flowmeter, suction filtration cylinder, vacuum pump and conduit, sample separation and concentration part include ultrasonic generator, sample
Bottle, flotation pipe, stirring rod and multi-stage screening disk, the glass part port in device are all ground production, can be between each section
Row arbitrarily disassembly assembling.Wherein, the liquid storage bottle is connected with the branch mouth for filtering cylinder bottom by a conduit with tongs
It connects;A conduit is placed in liquid storage bottle and is connect on peristaltic pump, flowmeter is provided among conduit, to control flotation fluid
The other end of flow velocity, conduit imports sample bottle bottom of bottle;Cylinder will be filtered to be placed in ultrasonic generator;Sample bottle is placed again
In filtering in cylinder, successively the sequence of flotation pipe from bottom to top is assembled on sample bottle, if finally dry sieving disk is nested in floating
It selects on the outside of pipe;Stirring rod is protruded into sample bottle;Finally the branch mouth for filtering cylinder top is connected with vacuum pump, the screening
The strainer or filter membrane of different-grain diameter are placed in disk, to realize the screening separation and enrichment of micro- plastic target object.
Further, the deposit sample that prior optimization processing is crossed is placed in sample bottle, suitable flotation fluid is added, opened
Stirring rod and ultrasonic wave can be such that sample uniformly mixes with flotation fluid, form suspension.
Further, the frequency range of the ultrasonic generator is 300MHz~500MHz.
Further, flotation liquid medium is sodium chloride, the saturated solution of sodium iodide or zinc chloride and degradable surface-active
Agent salting liquid, and the connection between liquid storage bottle and suction filtration cylinder, are recycled flotation fluid, reduce economic cost, and avoid
Cause secondary environmental pollution.
Further, the setting of disk is sieved, can according to actual needs, it can be to micro- plastics progress of different size in deposit
Quick continuous separation and concentration.The filter membrane or strainer of different-grain diameter are replaced according to demand, and e.g., in seabeach area, deposit includes
Micro- plastic grain aperture is larger, and aperture may be selected in the strainer of 4~200 mesh ranges;And in water body, nanometer ruler may be contained
Aperture may be selected in the filter membrane of 0.45~335 μ m in very little micro- plastic grain object.
Further, the number of screening disk (10) determines (the flotation pipe of every 10cm long according to the length of flotation pipe (8)
Locate settable screening disk, sufficiently long flotation pipe is to allow suspension is very fast, preferable on screening disk to separate).
Further, the assembling mode between the flotation fluid cyclic part and the separation and concentration part of sample be can be into
Row disassembly assembling, is convenient for carrying.
Further, ultrasonic wave is opened, is conducive to falling off for micro- frosting load substance, so as to the separation of micro- plastics.
Further, the screening disk is divided into upper, middle and lower-ranking, the strainer of replaceable different-grain diameter in the screening disk
Or filter membrane, so that micro- plastics of variable grain carry out continuous separation and concentration step by step, general principle is that upper layer places 4~80
100~200 mesh filter screens are placed in mesh filter screen, middle layer, and 0.45~335 μm of filter membrane is placed by lower layer.
Further, palpiform is put at sealing device, and on undermost screening disk between lower layer's screening disk and suction filtration cylinder
Filter membrane is set, when flotation fluid and micro- plastics arrival lower layer screening disk, reduced vacuum pump is opened and carries out decompression suction filtration, be convenient for tiny mud
The husky and micro- plastics of nanoscale are separated with flotation fluid, to achieve the purpose that the double purification of flotation fluid.
Further, for the double purification purpose of flotation fluid, it can be sieved in disk in lower layer and place filter membrane, this ensure that
Tiny micro- plastic grain of silt and nano-grade size and separating for flotation fluid.
Further, while opening vacuum pump, it is that the flotation fluid filtered in cylinder is recycled to that tongs, which are also required to open,
In liquid storage bottle.
A kind of application method for the enriching apparatus quickly continuously separating micro- plastics, which is characterized in that including following method:
(1) device assembles: the suitable experiment table top of selection first assembles each section, installation is first left and then right and under respectively
Principle on and is assembled, then each section is connected to become an entirety by conduit;
(2) leakproofness of check device: being added suitable distilled water in sample bottle and in liquid storage bottle, opening device, into
Row checks the reading of vacuum pump, to guarantee its normal use;
(3) sample-adding: being added processed sediment sample in advance in sample bottle, and flotation fluid turn on agitator is added and surpasses
Sound wave generating device mixes sample and flotation fluid uniformly, forms suspension;
(4) screening of micro- plastics: opening peristaltic pump, the flotation fluid in liquid storage bottle be pumped into sample bottle, adjusts stream
Meter enters flotation fluid in sample bottle with constant speed in the range of 1~3mL/min, to guarantee suspension slowly from floating
The top of pipe is selected to overflow, by sieving disk;When suspension reaches undermost screening disk, vacuum pump is opened, will include tiny
The flotation fluid of silt and the micro- plastics of nanoscale is quickly separated;Finally, opening tongs makes flotation fluid liquid storage bottle and pumping again
It is recycled between filter cylinder, is enriched with its micro- plastic grain in different screening disks;
(5) cleaning of micro- plastics: being replaced with deionized water for flotation fluid again, to guarantee that removal is adsorbed on micro- frosting
Flotation fluid solute collects micro- plastic grain of different-grain diameter, drying, in case detection respectively.
Compared with prior art, present invention has an advantage that
1) selection of flotation fluid is carried out according to the physicochemical property on existing flotation fluid preparation basis and sample, flotation fluid follows
Ring uses, and further reduces the cost of economic cost and secondary treatment waste liquid;
2) ultrasonication sample is selected, to be preferably that the sundries that the persistence of micro- frosting deposits removes, benefit
In obtaining original micro- plastic grain;
3) purpose of multilayer screening riddle point is selected, it, can be with convenient for disposably separating micro- plastics of variable grain
Efficiently carry out the enrichment of micro- plastics concentration;
4) use of vacuum pump improves the substance of nano-grade size and the separative efficiency of flotation fluid, can also be further rich
Collect the micro- plastic grain of nanoscale;
5) apparatus of the present invention are of simple structure and low cost, be easily assembled to and are easy to carry about with one that mobile, separative efficiency is high, realize
Continuous, the quick separation and concentration of micro- plastic grain of different size in deposit, and convenient for promoting the use of.
Detailed description of the invention
Fig. 1 is a kind of enriching apparatus schematic diagram for quickly continuously separating micro- plastics of the present invention;
Fig. 2 is flotation pipe (left side) and screening disk (right side) schematic diagram of the invention;
Fig. 3 is suction filtration cylinder schematic diagram of the invention.
All parts are as follows in figure: peristaltic pump 1, liquid storage bottle 2, flowmeter 3, tongs 4, ultrasonic generator 5, sample
Bottle 6 filters cylinder 7, flotation pipe 8, stirring rod 9, screening disk 10, vacuum pump 11, conduit 12.
Specific embodiment
The present invention will be further specifically described in detail with reference to specific embodiments, but embodiments of the present invention are not
It is limited to this, for not specifically specified technological parameter, can refer to routine techniques progress.
As shown in FIG. 1 to 3, the separation and concentration of micro- plastics fills in a kind of deposit based on the design of Density Separation principle
It sets, the continuous separation of the recycling of flotation fluid and the micro- plastic grain of different-grain diameter.Including flotation fluid cyclic part and sample point
From enriching section;The flotation fluid cyclic part includes peristaltic pump 1, liquid storage bottle 2, flowmeter 3, filters cylinder 7, vacuum pump 11 and lead
Pipe 12, sample separation and concentration part include ultrasonic generator 5, sample bottle 6, flotation pipe 8, stirring rod 9 and multistage sieve
Divide disk 10, the glass part port in device is all ground production, can arbitrarily be dismantled assembling between each section.Wherein,
The liquid storage bottle 2 is connected with the branch mouth for filtering 7 bottom of cylinder by a conduit 12 with tongs 4;It is placed in liquid storage bottle 2
A piece conduit 12 and connect on peristaltic pump 1, flowmeter 3 be provided among conduit, to control the flow velocity of flotation fluid, conduit it is another
One end imports 6 bottom of bottle of sample bottle;Cylinder 7 will be filtered to be placed in ultrasonic generator 5;Sample bottle 6 is placed in again and filters cylinder 7
In, successively the sequence of the flotation pipe 8 of long 30cm from bottom to top is assembled on sample bottle 6, if finally that dry sieving disk 10 is nested
In 8 outside of flotation pipe;The stirring rod 9 of one root long 40cm is protruded into sample bottle 6;Finally by the branch mouth on suction filtration 7 top of cylinder and very
Sky pump 11 is connected, and the strainer or filter membrane of different-grain diameter is placed in the screening disk 10, to realize micro- plastic target object
Screening separation and enrichment.The frequency range of the ultrasonic generator 5 is 300MHz~500MHz.Flotation liquid medium is chlorine
Change the saturated solution and degradable surfactant salting liquid of sodium, sodium iodide or zinc chloride, and liquid storage bottle 2 and filter cylinder (7) it
Between connection, flotation fluid is recycled, reduces economic cost, and avoids and causes secondary environmental pollution.Described is floating
Selecting the assembling mode between liquid cyclic part and the separation and concentration part of sample is that can carry out disassembly assembling, is convenient for carrying.It is described
Screening disk 10 divides for upper, middle and lower-ranking, the strainer or filter membrane for sieving replaceable different-grain diameter in disk 10, so as not to same
Micro- plastics of grain carry out continuous separation and concentration step by step, and general principle is that 4~80 mesh filter screens are placed on upper layer, and middle layer places 100
0.45~335 μm of filter membrane is placed by~200 mesh filter screens, lower layer.
The separation method of micro- plastic selector separation micro- plastics of different size, step include such as in a kind of deposit
Under:
1) the good saturated density flotation fluid of configured in advance is added in liquid storage bottle, then a certain amount of prior pretreated will must sunk
Product object is placed in sample bottle
Wherein, since the density of seawater is 1.03*103kg/m3, the flotation fluid density that selects here is greater than the density of seawater.
The principle for not causing according to economy and secondary pollution, is typically chosen saturated sodium-chloride and IodineSodium Solution, meanwhile, it can select
The solution of biodegradable surfactant salt, such as sophorolipid and rhamnolipid solution, so as to some loads of micro- frosting
Object carries out degradation and falls off.
Wherein, the key step of deposit processing, weighs the deposit of 500g, dries in 105 DEG C of baking oven, be placed in mortar
Middle grinding carries out screening process using the steel sieve in the aperture 10mm, obtains deposit A;Deposit A300g is weighed again, is added dropwise
Behind hydrogen peroxide dipping 3~5 hours of 30mL 30%, it is dried, it is spare.
2) it opens peristaltic pump and adjusts flowmeter, the flotation fluid for being put into 200mL with the speed of 3mL/min is closed in sample bottle
Peristaltic pump is closed, stops flotation fluid and enters in sample bottle;
3) it filters again and a small amount of flotation fluid is also added in cylinder, open ultrasonic wave and stirring rod, make flotation fluid and separation sample
Sufficiently become suspension;
Further, the ultrasonic wave of 300W is selected to be ultrasonically treated in above-mentioned steps, the mixing speed control of stirring rod
In 80rpm.
4) about after 15min, it is again turned on peristaltic pump, flowmeter is adjusted, flotation fluid is made to be pumped into sample with the speed of 1.0mL/min
Product bottom of bottle portion, the suspension with frivolous substance slowly float, and at this moment suspension is slowly overflowed from the top of flotation pipe;
5) when suspension by top nozzle spilling after, first reach upper layer large aperture strainer on be filtered, compared
Relatively large micro- plastic grain MPs1, suspension continues to flow down later, carries out the secondary of micro- plastic grain by intermediate strainer
Separation, obtains micro- plastics MPs2 of medium grain;
Further, the aperture of the sieve in upper middle layer should be controlled in 5mm >=R≤0.45 μm.
6) when suspension reaches on undermost filter membrane, opening vacuum pump makes tiny silt and micro- plastics in suspension
Grain is quickly filtered out, wherein obtaining micro- plastic grain MPs3 of some nano-grade sizes;
Further, filtering the flotation fluid liquid level in cylinder must not exceed 2/3rds of filtrate cylinder, reach 2/3rds
When left and right, tongs are opened, so that flotation fluid is flowed into liquid storage bottle from suction filtration cylinder, prevents flotation fluid to be drawn into vacuum pump, together
When, flotation fluid is recycled.
7) by the flotation fluid in liquid storage bottle alternatively at deionized water or other cleaning solution, according to 1)~6) step into
Washing of the row to micro- plastic sample, then the sample on different screening disks is air-dried into processing, it saves, in case test uses.
Further, in above-mentioned steps, in the cleaning process of micro- plastics, the circulation time of cleaning solution should be controlled
Between 3~5h;Isolated micro- plastics should be handled using natural air drying.
Embodiment 1
The bottom sediment that certain mechanism is acquired in CHINESE OFFSHORE near zone choose 5 sampled points (S1, S2, S3, S4,
S5) weigh respectively 500g crude product be placed on surface plate air-dry, remove stone, biomass and the sundries of bulk, obtain deposit A;
Deposit A is placed in mortar and is ground, screening is sieved using the big steel in the aperture 5~10mm, obtains deposit B;Weigh deposit
The stirring of 10mL deionized water is added in beaker, the hydrogen peroxide of 20mL 30% is slowly added dropwise, wait react about in beaker by B300g
It after 3 hours, is placed in 80 DEG C of baking oven and dries, grind, obtain deposit C, as the sediment sample for sieving micro- plastics.Flotation
The preparation of liquid: at room temperature, the sodium chloride solution of saturation, and the rhamnolipid aqueous solution of alkalinity is configured, is mixed with the ratio of 8:2
It is spare as flotation fluid.
As shown in Figure 1, the sediment sample handled well in advance to be separated is added in sample bottle 6, infused in liquid storage bottle
Full flotation fluid, the flotation fluid of injected slurry volume about a quarter in bottle,suction, the flow velocity for opening peristaltic pump and adjusting flowmeter make
Flotation fluid is after about 200mL, to stop injection flotation fluid in the speed of 3mL/min injection sample bottle, and opening ultrasonic wave, (power is
300W) with stirring rod (revolving speed 80rpm), deposit C and flotation fluid is made to be thoroughly mixed to form suspension A, after stirring 15min.
Peristaltic pump is opened, adjusting flowmeter injects flotation fluid in sample bottle with the speed of 1.0ml/min, and adjusts stirring
The revolving speed of stick is 30rpm, and the suspension A being diluted at this time is slowly floated with constant speed, and the top for reaching flotation pipe is overflowed.
Further, the suspension of spilling is successively by the screening disk of upper layer (20 mesh screen) and middle layer (100 mesh screen),
Obviously there is particulate matter to be filtered out at this time to come, be designated as particulate matter 1 and 2, in the screening by lowest level (0.45 μm of filter membrane)
When disk, vacuum pump is opened, the tiny particles content in suspension is filtered quickly, stays on filter membrane, be designated as particulate matter 3.
Further, when filter cylinder in flotation fluid reach 3/4ths of volume when, open tongs, make flotation fluid with
Constant flow velocity recycles between liquid storage bottle and suction filtration cylinder.
Flotation fluid in liquid storage bottle 10 is replaced with into deionized water, opens peristaltic pump 1, the flow for adjusting flowmeter is 10mL/
Min, and vacuum pump and tongs are opened, make deionized water with constant flow rate by three layers of screening disk, online of cleaning screen
The particulate matter cleaned up is carried out air-drying processing, be observed through Stereo microscope, the quantity of products therefrom such as the following table 1 by grain object, and
Infrared spectroscopy, Raman spectrum and scanning electron microscope characterization test are carried out to these particulate matters, wherein upper layer, middle layer and lower layer sieve
Divide the particulate matter for all having obtained micro- plastics in disk, is mainly transparent plastic, has by the discovery of the characterizations such as infrared spectroscopy, Raman spectrum
Color plastics, glass fibre etc..
Table 1, the product number (being counted under Stereo microscope) for micro- plastic grain that five sampled points are obtained by screening
S1 | S2 | S3 | S4 | S5 | |
Upper layer disc () | 3 | 0 | 0 | 8 | 1 |
Middle layer disk () | 18 | 32 | 19 | 26 | 38 |
Lower layer's disk (g) | 0.023 | 0.004 | 0.018 | 0.001 | 0.043 |
Embodiment 2
By the linear low density polyethylene particle (partial size about 2~3mm or so) of purchase, 2.04g is weighed, in Stereo microscope
Lower counting has 85, is added in the beaker for filling the 250mL of 300g soil, is uniformly mixed, as simulation sediment sample.
The simulation sediment sample of preparation is added in sample bottle;The flotation fluid of preparation is saturated sodium chloride solution;Sieve
Selection be upper layer sieve disk (40 mesh screen), middle layer sieve disk (not putting) and lower layer screening disk (room ordinary filter paper), obtain
Sample drying and processing in 80 DEG C of baking oven, other operating procedures and embodiment 1 are consistent.
Micro- plastic grain of 2.09g is always obtained in final three layers of screening, observation counts 85 under Stereo microscope, by it
Obtained plastic grain drying, processing.The rate of recovery of its sample reaches 100%, wherein without micro- modeling in middle layer, lower layer's screening disk
Expect particle.
Embodiment 3
By the polypropylene plastics particle (2~3mm of partial size) of purchase, 1.54g is weighed, is added in pulverizer and is crushed
Its resulting plastic crushing particulate matter is all added in the beaker for filling the 250mL of 300g soil by 5min, is uniformly mixed,
As simulation sediment sample.
The simulation sediment sample of preparation is added in sample bottle;The flotation fluid of preparation is saturated sodium chloride solution;Sieve
Selection be upper layer sieve disk (40 mesh screen), middle layer sieve disk (100 mesh screen) and lower layer screening disk (0.45 μm of filter membrane),
Other operating procedures and embodiment 1 are consistent.
Micro- plastic grain of 1.46g is always obtained in final three layers of screening, the rate of recovery of sample reaches 94.8%, wherein
It includes fraction of silt that lower layer, which sieves in micro- plastic grain in disk,.
Claims (9)
1. a kind of enriching apparatus for quickly continuously separating micro- plastics, which is characterized in that including flotation fluid cyclic part and sample point
From enriching section;The flotation fluid cyclic part includes peristaltic pump (1), liquid storage bottle (2), flowmeter (3), filters cylinder (7), vacuum
Pump (11) and conduit (12);Sample separation and concentration part includes ultrasonic generator (5), sample bottle (6), flotation pipe
(8), stirring rod (9) and multi-stage screening disk (10);Wherein, the branch mouth of the liquid storage bottle (2) and suction filtration cylinder (7) bottom is by a band
There is the conduit (12) of tongs (4) to be connected;A conduit (12) is placed in liquid storage bottle (2) and is connect on peristaltic pump (1), is led
Flowmeter (3) are provided among pipe, to control the flow velocity of flotation fluid, the other end of conduit imports sample bottle (6) bottom of bottle;It will take out
Filter cylinder (7) is placed in ultrasonic generator (5);Sample bottle (6) is placed in again and is filtered in cylinder (7), successively flotation pipe
(8) sequence from bottom to top is assembled on sample bottle (6), if finally dry sieving disk (10) is nested on the outside of flotation pipe (8);It will
Stirring rod (9) protrudes into sample bottle (6);Finally the branch mouth for filtering cylinder (7) top is connected with vacuum pump (11), the sieve
Divide the strainer or filter membrane that different-grain diameter is placed in disk (10), to realize the screening separation and enrichment of micro- plastic target object.
2. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: the ultrasonic wave occurs
The frequency range of device (5) is 300MHz~500MHz.
3. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: flotation liquid medium is chlorine
One or more of change sodium, the saturated solution of sodium iodide or zinc chloride and degradable surfactant salting liquid;Liquid storage bottle (2) with
The connection between cylinder (7) is filtered, flotation fluid is recycled, reduces economic cost, and avoids and causes secondary environment dirty
Dye.
4. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: the screening disk (10)
Number determined according to the length of flotation pipe (8), one screening disk of setting, sufficiently long flotation pipe at the flotation pipe of every 10cm long
It is to allow suspension is very fast, preferable on screening disk to separate.
5. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: the flotation fluid follows
Assembling mode between loop section and the separation and concentration part of sample is that can carry out disassembly assembling, is convenient for carrying.
6. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: it opens ultrasonic wave (5),
Be conducive to falling off for micro- frosting load substance, so as to the separation of micro- plastics.
7. quickly continuously separating the enriching apparatus of micro- plastics according to claim 1, it is characterised in that: the screening disk (10)
It is divided into upper, middle and lower-ranking, the strainer or filter membrane of replaceable different-grain diameter in screening disk (10) are micro- so as to variable grain
Plastics carry out continuous separation and concentration step by step, and general principle is that 4~80 mesh filter screens are placed on upper layer, and middle layer places 100~200
0.45~335 μm of filter membrane is placed by mesh filter screen, lower layer.
8. quickly continuously separating the enriching apparatus of micro- plastics according to claim 7, it is characterised in that: disk (10) are sieved by lower layer
Palpiform places filter membrane at sealing device, and on undermost screening disk (10) between suction filtration cylinder (7), when flotation fluid and micro- modeling
Expect that unlatching reduced vacuum pump (11) carries out decompression suction filtration when sieving disk (10) up to lower layer, it is micro- convenient for tiny silt and nanoscale
The separation of plastics and flotation fluid, to achieve the purpose that the double purification of flotation fluid.
9. the application method of any one of claim 1~8 enriching apparatus for quickly continuously separating micro- plastics, feature exist
In, including following method:
(1) device assembles: each section first being assembled respectively, first left and then right and from bottom to top principle is installed and is assembled, then lead to
It crosses conduit and each section is connected to become an entirety;
(2) leakproofness of check device: in sample bottle and suitable distilled water is added in liquid storage bottle, opening device is examined
The reading of vacuum pump is looked into, to guarantee its normal use;
(3) it is loaded: processed sediment sample in advance being added in sample bottle, flotation fluid turn on agitator and ultrasonic wave is added
Generating device mixes sample and flotation fluid uniformly, forms suspension;
(4) screening of micro- plastics: opening peristaltic pump, the flotation fluid in liquid storage bottle be pumped into sample bottle, adjusts flowmeter
Enter flotation fluid in sample bottle with constant speed in the range of 1~3mL/min, to guarantee suspension slowly from flotation pipe
Top overflow, pass through screening disk;When suspension reaches undermost screening disk, vacuum pump is opened, will include tiny silt
It is quickly separated with the flotation fluid of the micro- plastics of nanoscale;Finally, opening tongs makes flotation fluid liquid storage bottle and suction filtration cylinder again
Between be recycled, be enriched with its micro- plastic grain in different screening disks;
(5) cleaning of micro- plastics: being replaced with deionized water for flotation fluid again, to guarantee that removal is adsorbed on the flotation of micro- frosting
Liquid solute collects micro- plastic grain of different-grain diameter, drying, in case detection respectively.
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