CN107367449A - Traceable PM2.5 particulate composites and preparation method thereof - Google Patents
Traceable PM2.5 particulate composites and preparation method thereof Download PDFInfo
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- CN107367449A CN107367449A CN201710629470.8A CN201710629470A CN107367449A CN 107367449 A CN107367449 A CN 107367449A CN 201710629470 A CN201710629470 A CN 201710629470A CN 107367449 A CN107367449 A CN 107367449A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 230000006378 damage Effects 0.000 claims abstract description 6
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- 238000004088 simulation Methods 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract 2
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- 238000006243 chemical reaction Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229920000858 Cyclodextrin Polymers 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229910007486 ZnGa2O4 Inorganic materials 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010382 chemical cross-linking Methods 0.000 claims description 3
- 238000009766 low-temperature sintering Methods 0.000 claims description 3
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
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- 239000000126 substance Substances 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 230000035515 penetration Effects 0.000 abstract description 4
- 239000012620 biological material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 8
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- 241001465754 Metazoa Species 0.000 description 2
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- 210000000056 organ Anatomy 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
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- 238000001218 confocal laser scanning microscopy Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 239000012188 paraffin wax Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/075—Investigating concentration of particle suspensions by optical means
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a kind of traceable PM2.5 particulate composites and preparation method thereof, and the PM2.5 particles and nano luminescent particles that are collected into air are obtained into traceable PM2.5 particulate composites using compound method is chemically crosslinked.These materials with micro nano structure, can be as the biomaterial and functional material of the formation of haze, harm, defence simulation and pathological study, for association area with the performance such as stable luminescent property, traceable, high biological penetration.
Description
Technical field
The invention belongs to technical field of biological material, more particularly to a kind of traceable haze particulate composite and its preparation side
Method, the method that PM2.5 particles are specifically chemically crosslinked using luminescent material, prepare the haze of traceable high-penetration ability
Grain, simulation and pathological study are defendd for haze.
Background technology
With the rapid expansion of China's economic scale and the quickening of urbanization process, atmospheric aerosol pollution is on the rise,
Visibility deterioration event is also more and more as caused by aerosol, haze turn into endanger mankind's publilc health major reason it
One, particularly PM2.5 particles.NO in PM2.5 particles3-,SO4 2-, Cl-,NH4+,Na+The more normal airborne particulate of plasma concentration
Height, major pollutants are the heavy metals such as As, Cr, PB, Ti and V, so into human organ can be damaged after human body.So PM2.5
How specific intrusion feature isHow PM2.5 damage human organ and system are defenddThese problems receive much concern always.Solution
Certainly can the key of problem be clearly to mark the route map that human body is invaded and discharged with tracer PM2.5 particles.
Up-conversion luminescence, refer to that material absorbs the photon (being usually near infrared light) of two or more low energy and launched
The process of the photon (being usually visible ray) of high-energy.It is long-persistence luminous, refer to material after stopping is excited, it is luminous still to be able to hold
Continuous a period of time, the duration that lights is from several seconds to several weeks.Up-conversion luminescence nano particle and near-infrared long afterglow are received
Rice grain causes the extensive concern of people as nanocomposite optical probe for biological in-vivo imaging.Because upper conversion hair
Photoimaging be typically using 980nm near infrared lights as excitation source, and near-infrared long afterglow be imaged be then using near infrared light as
Imaging signal.In imaging process, either using near infrared light as excitation source or imaging signal, can greatly it drop
The ambient interferences (such as autofluorescence) of low bio-tissue, so as to significantly improve tissue penetration depths of bio-imaging and sensitive
Degree.
At present, because PM2.5 hazes particle composition is complicated, has certain pathogenic and toxicity, therefore, prior art one
As the process of human body invaded PM2.5 hazes particle by type material study, but type material prepares complicated, fidelity
It is not high, its extensive use is limited, therefore, is badly in need of a kind of more simple, efficient PM2.5 particles tracing method.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of nano luminescent material and PM2.5 haze particulate composites
Preparation method, i.e., conversion or long after glow luminous material chemical crosslinking PM2.5 particles in nanometer.When particle enters lung tissue,
By the mark to particle and tracer, research PM2.5 particles are prevented PM2.5 particles the phagocytic process and tissue of human body
Imperial mechanism, the results showed that：This method can clearly mark the route map that human body is invaded and discharged with tracer PM2.5 particles.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of traceable PM2.5 particulate composites, including：
PM2.5 haze particles；
The nanophosphors particle being coated on PM2.5 haze particles；
The traceable PM2.5 particulate composites are core shell structure；
The PM2.5 hazes particle is by immersion, drying process.
In order to overcome present mode material to prepare the problem of complicated, fidelity is not high, the present invention devises one kind and can lighted
PM2.5 particles, it is irregular using PM2.5 haze grain shapes, the characteristics of easy contaminant-laden, will be changed in nanometer or it is long more than
Brightness luminescent material is coated on outside it, forms tracer body.The complete of PM2.5 haze grain structures has not only been effectively ensured in this method
Property, the ambient interferences that PM2.5 particles invade bio-tissue during human body are also greatly reduced, significantly improve the group of imaging
Knit penetration depth and sensitivity.
Preferably, the mass fraction of the PM2.5 hazes particle can be 0.1-99.9%.
Present invention also offers a kind of preparation method of traceable PM2.5 particulate composites, including：
PM2.5 haze particles are collected, are soaked in organic solvent, are freeze-dried, it is stand-by；
By nanophosphors particle and PM2.5 haze particles mixed grinding in the presence of chemical cross-linking agent, must mix
Grain, dry, low-temperature sintering, produce traceable PM2.5 particulate composites.
In order to obtain a kind of simple, tracer effect preferably PM2.5 particulate composites preparation method, the present invention is not to
With under combination, PM2.5 particles and nanophosphors material combination rule and and its influence to tracer effect carry out
System research, found after large scale experiment is groped：Haze particle after freeze-dried is with nano luminescent particles in chemistry
Under glue crosslinking agent effect, it can be formed with the traceable PM2.5 particles of shell full-package structure through drying, low-temperature sintering.This method has
It is easily controlled, simple process, passes through the parameters such as control proportioning both controllable traceable PM2.5 particulate composites
Size and performance, and tracer effect is more excellent.
Preferably, the nanophosphors particle is ZnGa2O4：Cr3+Deng long after glow luminous material, NaYF4：Yb3+, Er3 +Deng up-conversion luminescent material.
Preferably, the PM2.5 particles are that mass ratio is 1000 with nanophosphors grain mixture ratio：1~1：1000.
Preferably, the organic solvent is the organic solvents containing hydroxyl such as ethanol, methanol.
Preferably, the chemical glue crosslinking agent be polyvinyl alcohol (PVA), cyclodextrin, paraffin etc. can biologic applications organic modeling
Agent.
Preferably, the drying is freeze-drying, and condition is：Cryogenic temperature is -200 DEG C, freezes 50h, fully dries.
Present invention also offers traceable PM2.5 particulate composites prepared by any above-mentioned method.
Luminescent nanoparticle and PM2.5 particles are chemically crosslinked by the present invention, utilize Illuminant nanometer material high sensitivity, Gao Wen
It is qualitative to wait superior luminescence performance and biological tracing performance to prepare traceable PM2.5 particulate composites with PM2.5 Particles disperseds, obtain
Obtain controllable size, uniformly compound, stable, traceable, the high biological penetration of property PM2.5 particles, the shape for haze
Into, harm, defence simulation and pathological study.
Present invention also offers any above-mentioned traceable PM2.5 particulate composites in the tracer of haze particle and haze
Formed, the application in harm, defence simulation and pathological study.
Because intake is few and is mainly used in scientific research, therefore, traceable PM2.5 particulate composites of the invention are to people
The injury of body and animal can be neglected.If necessary, mark and the tracer of cell culture can be only used for.
Beneficial effects of the present invention
(1) traceable PM2.5 particulate composites provided by the invention and preparation method thereof, be using conversion in nanometer or
Long after glow luminous material is chemically crosslinked PM2.5 haze particles.The present invention has prepared traceable PM2.5 particulate composites.This
Invention devises a kind of can have traceable, high-penetration ability, can solve the problems, such as tracer with the PM2.5 particles of luminescence generated by light
And probe into the route of go the rounds of haze particle in animal body, i.e., directly observe biology using traceable PM2.5 particulate composites
Organize the defence to haze particle and invasion mechanism.
(2) in the present invention, different luminescent material performances, different tracers are prepared by choosing different luminescent materials
The PM2.5 composites of matter.By controlling the different ratio of luminescent material and haze particle to prepare various PM2.5 contents, hair
The traceable PM2.5 composites of brightness.PM2.5 mass fraction can be 0.1- in traceable PM2.5 composites
99.9%.
(3) preparation method of the present invention is simple, luminous efficiency is high, practical, easy to spread.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not form the improper restriction to the application.
Fig. 1 is embodiment 1PM2.5 and ZnGa2O4：Cr3+Glue joins composite construction.
Fig. 2 is the Elemental redistribution structure of the traceable PM2.5 particulate composites of embodiment 1.
Fig. 3 is embodiment 1ZnGa2O4：Cr3+Emission in Cubic particles coat PM2.5 granulated shelling clad structures it is traceable
PM2.5 particulate composites.
Fig. 4 is the photoluminescence performance of the traceable PM2.5 particulate composites of embodiment 1.
Fig. 5 is the afterglow property of the traceable PM2.5 particulate composites of embodiment 1.
Fig. 6 is the traceable PM2.5 particulate composites Laser Scanning Confocal Microscope image of embodiment 4.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
Embodiment 1：
1) air collector (MH1200, atmosphere particulate matter sampler, Yancheng Tian Yue instrument and meters Co., Ltd) will be used to receive
Collected PM2.5 haze particles glass fiber filter be dipped into ethanol soak 12h after filter membrane is taken out, will be dissolved with PM2.5
The ethanol solution of grain is placed in vacuum freezing drying oven, and (Scientz-ND, freeze drier, the new sesame biotechnology share in Ningbo are limited
Company), it is -200 DEG C to set cryogenic temperature, freezes 50h, abundant evaporation drying, the PM2.5 particles after being handled；
2) ZnGa for preparing solid phase method2O4：Cr3+Dissolved after (according to patent CN201510650991.2) stirring, ultrasound
Into water, stand 24 hours, take suspension, with centrifuge in the case where revolution is 10000rpm high speed centrifugation, you can average grain is made
The luminous ZnGa of near-infrared overlength afterglow of the footpath less than 100nm2O4：Cr3+Nano particle.
3) ZnGa is taken2O4：Cr3+Nano particle 0.02g, PM2.5 particle 0.02g and the 0.25g cyclodextrin after processing are common
It is dissolved in 60ml water, is stirred vigorously in three-necked flask under nitrogen protection to being completely dissolved, adds 1mol/L NaOH regulations pH
For 9-10, obtained dark solution is poured into flask ultrasonic reaction 1h, 24h is dried in vacuo, obtains dry particle；
4) it is that cyclodextrin decomposes volatilization the dry particle obtained in 3) to be sintered to 4h at 300 DEG C to carry out degummings volatilization, is obtained
To traceable PM2.5 particulate composites；
With the structure and composite of particle after ESEM (SEM, TDCLS-4800, Toshiba Corp) observation glue connection
Structure, such as Fig. 1,3.Composite particles structure, such as Fig. 2 are observed with X-ray energy spectrum (EDS, TDCLS-4800, Toshiba Corp).
With sepectrophotofluorometer (F-7000,200-900nm, HIT) test analysis composite photoluminescence performance,
Such as Fig. 4 and afterglow property, such as Fig. 5.
Embodiment 2：
Using the identical method of embodiment 1, cyclodextrin used in the polyvinyl alcohol replacement that use quality fraction is 5%,
Traceable PM2.5 particulate composites are made.
The traceable PM2.5 particulate composites for taking the embodiment to prepare characterize sample property, testing result and embodiment 1
It is close.
Embodiment 3：
Using the identical method of embodiment 1, with near-infrared long after glow luminous material Zn3Ga2Ge2O10:Cr3+(according to patent
CN103215041A compound, obtained traceable PM2.5 particulate composites) are carried out with PM2.5 particles.
The traceable PM2.5 particulate composites for taking the embodiment to prepare characterize sample property, testing result and embodiment 1
It is close, and traceable PM2.5 particulate composites long afterglow performance is more preferably.
Embodiment 4：
Using the identical method of embodiment 1, with up-conversion luminescent material NaYF4：Yb3+, Er3+(according to patent
CN105112056A compound, obtained traceable PM2.5 particulate composites) are carried out with PM2.5 particles.
The traceable PM2.5 particulate composites for taking the embodiment to prepare characterize sample property, testing result and embodiment 1
It is close, and traceable PM2.5 particulate composites have up-conversion luminescence performance.
Embodiment 5：
Using the identical method of embodiment 1, by ZnGa2O4：Cr3+With haze particle according to mass ratio 10:1 ratio, can
Tracer PM2.5 particulate composites.
The traceable PM2.5 particulate composites for taking the embodiment to prepare characterize sample property, testing result and embodiment 1
It is close.
Embodiment 6：
Using the identical method of embodiment 1, by ZnGa2O4：Cr3+With haze particle according to mass ratio 20:1 ratio, can
Tracer PM2.5 particulate composites.
The traceable PM2.5 particulate composites for taking the embodiment to prepare characterize sample property, testing result and embodiment 1
It is close.
Embodiment 7：
Traceable PM2.5 particulate composites are prepared using the identical method of embodiment 4, are swashed to be equipped with Ti∶Sapphire laser pulse
The Laser Scanning Confocal Microscope of light is imaged (CLSM, AZ-C2+, Japanese Nikon Co., Ltd.) observation composite it is near in 980nm
520-540nm visible ray, such as Fig. 6 are sent under infrared ray excited.It can be inferred that when the composite is used for cell culture and life
During object culture, Laser Scanning Confocal Microscope and living imaging instrument (DS-Ri1-U3Digital Camera, Japanese Nikon strains can be passed through
Formula commercial firm) it is marked and tracer.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. traceable PM2.5 particulate composites, it is characterised in that including：PM2.5 haze particles；The nanophosphors particle being coated on PM2.5 haze particles；The traceable PM2.5 particulate composites are core shell structure；The PM2.5 hazes particle is by immersion, drying process.
- 2. material as claimed in claim 1, it is characterised in that the mass fraction of the PM2.5 hazes particle can be 0.1- 99.9%.
- A kind of 3. preparation method of traceable PM2.5 particulate composites, it is characterised in that including：PM2.5 haze particles are collected, are soaked in organic solvent, are freeze-dried, it is stand-by；By nanophosphors particle and PM2.5 haze particles mixed grinding in the presence of chemical cross-linking agent, obtain hybrid particles, do Dry, low-temperature sintering, produce traceable PM2.5 particulate composites.
- 4. method as claimed in claim 3, it is characterised in that the nanophosphors particle is ZnGa2O4：Cr3+It is isometric remaining Brightness luminescent material, NaYF4：Yb3+, Er3+Deng up-conversion luminescent material.
- 5. method as claimed in claim 3, it is characterised in that the PM2.5 particles are with nanophosphors grain mixture ratio Mass ratio is 1000：1~1：1000.
- 6. method as claimed in claim 3, it is characterised in that the organic solvent is the having containing hydroxyl such as ethanol, methanol Solvent.
- 7. method as claimed in claim 3, it is characterised in that the chemical glue crosslinking agent be polyvinyl alcohol (PVA), cyclodextrin, Etc. can biologic applications organic plasticizer.
- 8. method as claimed in claim 3, it is characterised in that the drying is freeze-drying, and condition is：Cryogenic temperature for- 200 DEG C, 50h is freezed, is fully dried.
- 9. traceable PM2.5 particulate composites prepared by the method described in claim any one of 3-8.
- 10. the traceable PM2.5 particulate composites described in claim 1,2 or 9 any one are in the tracer of haze particle and haze Formation, harm, defence simulation and pathological study in application.
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