CN106943968B - A kind of preparation method of coding microball - Google Patents
A kind of preparation method of coding microball Download PDFInfo
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- CN106943968B CN106943968B CN201710203017.0A CN201710203017A CN106943968B CN 106943968 B CN106943968 B CN 106943968B CN 201710203017 A CN201710203017 A CN 201710203017A CN 106943968 B CN106943968 B CN 106943968B
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- 239000011806 microball Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 230000002035 prolonged effect Effects 0.000 claims abstract description 10
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 238000007711 solidification Methods 0.000 claims abstract description 5
- 230000008023 solidification Effects 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 claims description 12
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Natural products CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 9
- 239000004925 Acrylic resin Substances 0.000 claims description 8
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 8
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229920000728 polyester Polymers 0.000 claims description 5
- -1 thioxanthones Chemical compound 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical class C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims 1
- 239000012965 benzophenone Substances 0.000 claims 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 26
- 239000000523 sample Substances 0.000 abstract description 9
- 238000000018 DNA microarray Methods 0.000 abstract description 8
- 239000007791 liquid phase Substances 0.000 abstract description 7
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 7
- 125000004386 diacrylate group Chemical group 0.000 description 6
- 239000002096 quantum dot Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229960003638 dopamine Drugs 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229920006305 unsaturated polyester Polymers 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 206010001497 Agitation Diseases 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 150000008366 benzophenones Chemical class 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- DCAYPVUWAIABOU-NJFSPNSNSA-N hexadecane Chemical group CCCCCCCCCCCCCCC[14CH3] DCAYPVUWAIABOU-NJFSPNSNSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of preparation method of coding microball, include the following steps: that (1) mixes encoded material with aqueous oligomer, corresponding water-soluble photoinitiator dissolution is added completely, and vibrate and stir evenly, forms stable suspension as water phase；(2) alkanes solvent and emulsifier mixing shaken well are formed into oily phase；(3) water phase is instilled in the oily phase in stirring, the volume of the oil phase is 20-30 times of the water phase volume, the suspension system of even suspension is continued stirring until after dripping, and carry out ultraviolet light prolonged exposure to the suspension system；(4) after being washed the product after solidification for several times, the microballoon of target grain size is screened, obtains the coding microball after dry.The coding microball good hydrophilic property that preparation method of the present invention is prepared, coding efficiency is excellent, be easy to be surface modified with probe be grafted, so as to provide the coding microball carrier for having stable decoding capability for liquid phase biochip.
Description
Technical field
The invention belongs to analytical chemistry and technical field of molecular biology, it is related to a kind of having biomolecule identification function
The preparation of liquid phase biochip carrier coding microball, especially a kind of preparation method of coding microball.
Background technique
Liquid phase biochip technology be micro-nano magnitude spherical support surface carry out bioprobe grafting after, with to
Sample carries out hybridization reaction, detects the object information in sample to be tested, completes the analysis to sample to be tested.Compared to tradition
Solid base biochip, liquid phase biochip test high sensitivity, consumption sample amount is few, and biological affinity is high.A bit particularly important
To carry out hybridization reaction using different probe microballoon for same sample to be tested, can be completed at the same time same sample it is different at
The detection divided, that is, multi-channel detection.In the same reaction system, the performance of multi-channel detection is depended on to different beads
Identification, here it is the carrier microballoons encoding and decoding techniques of liquid phase biochip.In rapid development process, researchers' accumulation
Many coding means, from being based on Microsphere Size, the basic parameters such as shape to color, the spectrum encoding and decoding technique such as photonic crystal.
In these coding means, fluorescence spectrum encoding and decoding and laser induced breakdown spectroscopy encoding and decoding are application potential maximums, and are compiled
The code most excellent coding mode of effect.Fluorescence spectrum coding techniques is marked carrier microballoons using fluorescent material, passes through
The combination of different colours and intensity identifies microballoon on different microballoons.This coding mode can mention for liquid phase biochip technology
For enough recognizable carrier microballoons.Laser induced breakdown spectroscopy is a novel coding techniques, by various elements material
Material, especially on the Material cladding to microballoon containing metallic element, is excited using laser pulse, acquires coding microball plasma
The laser induced breakdown spectroscopy that bodyization generates, identifies atomic spectral line wherein included, so that it may verify element compound on microballoon
Type.Atomic spectral line spectral peak is sharp and stablizes readable, is digitally converted available number to laser induced breakdown spectroscopy
Change coding microball, this provides one revolutionary progress of coding microball.
In fluorescent material marks and laser induced breakdown spectroscopy Material cladding field, there is such as self-healings, electrostatic certainly
Assembling and it is micro-fluidic synthesis etc. various complex methods, but these modes all there is a problem of it is various.Such as: from
Matching of the coding mode that heals dependent on the bulk of encoded material and carrier microballoons, and requiring carrier is porous microsphere, this
Exclusion for subsequent non-specific adsorption increases difficulty.Electrostatic self-assembled require between encoded material and carrier electrically matching or
It needs to carry out more complicated surface modification, and composite effect is unstable.Micro-fluidic synthesis needs more accurate experiment condition
With stringent experimental implementation.The above complex method all can not provide the side of a set of universality for different encoded materials simultaneously
Case.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of preparation method of coding microball.
The technical solution adopted by the invention is as follows:
A kind of preparation method of coding microball, comprising the following steps:
(1) encoded material is mixed with aqueous oligomer, corresponding water-soluble photoinitiator dissolution is added completely, and vibrate and stir
It mixes uniformly, forms stable suspension as water phase；
(2) alkanes solvent and emulsifier mixing shaken well are formed into oily phase；
(3) water phase in step (1) is instilled in the oily phase in the step (2) in stirring, the oil phase
Volume is 20-30 times of the water phase volume, the suspension system of even suspension is continued stirring until after dripping, and to the suspension
System carries out ultraviolet light prolonged exposure；
(4) after being washed the product after solidification for several times, the microballoon of target grain size is screened, obtains institute after dry
State coding microball.
Preferably, in the step (3), the wavelength of the ultraviolet light is 355-375nm, irradiation energy 200-250mW.
Preferably, the encoded material includes fluorescence-encoded material and laser induced breakdown spectroscopy encoded material.
Preferably, the fluorescence-encoded material is semiconductor fluorescence quantum dot；The laser induced breakdown spectroscopy encodes material
Material is the nano material containing metallic element.
Preferably, the aqueous oligomer in the step (1) includes epoxy acrylic resin class, polyurethane acrylic resin
Class, polyester acrylate resin class, acrylated acrylics class and unsaturated polyester (UP) class；The aqueous initiator includes two
Benzophenone class, thioxanthones, diaryl phosphin be oxide-based and 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone.
Preferably, the aqueous oligomer in the step (1) is polyethyleneglycol diacrylate, the water-soluble photoinitiator
For 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone；In every milliliter of polyethyleneglycol diacrylate, 2- hydroxyl -4'-
The content of (2- hydroxy ethoxy) -2- methyl phenyl ketone is 10-30 milligrams.
Preferably, in the step (1), the alkanes solvent is hexadecane, and the emulsifier is cetyl polyethylene glycol,
The volume of the hexadecane is 15-25 times of the volume of the cetyl polyethylene glycol.
Preferably, in the step (3), the speed of stirring is 500-700 revolutions per minute, and the time persistently stirred is 1-
2 minutes, the time of the ultraviolet light prolonged exposure was 10-20 minutes.
Preferably, it in the step (4), is washed using hexamethylene and alcohol mixed solution；The hexamethylene and second
The volume ratio of alcohol is 2:1-1:2.
Preferably, in the step (4), the microballoon of target grain size is screened using stainless steel tm screen, it is described not
The size for steel tm screen of becoming rusty is -500 mesh of 400 mesh.
It compared with prior art, can be with one the beneficial effect comprise that of the invention is hydrophilic coding microball
Secondary property, in large quantity composite coding microballoon, substantially increase coding microball synthesis efficiency, reduce synthesis cost, effectively for
Different types of encoded material provides the synthetic method of universality, can be synthesized more using the bioaffinity of aqueous polymerization object
Add the coding microball suitable for biomolecule detection；It is low using material toxicity, pollution is small, preparation process is easy, safety, is conducive to
It is a wide range of to promote, and the coding microball good hydrophilic property that preparation method of the present invention is prepared, coding efficiency is excellent, is easy to carry out table
Face modification and probe grafting, so as to provide the coding microball carrier for having stable decoding capability for liquid phase biochip.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of coding microball obtained in the embodiment of the present invention 1；
Fig. 2 is the figure of coding microball obtained under the microscope in the embodiment of the present invention 1；
Fig. 3 is the decoding spectrum of coding microball obtained in the embodiment of the present invention 1；
Fig. 4 is the laser induced breakdown spectroscopy decoding spectrum of coding microball obtained in the embodiment of the present invention 2；
Fig. 5 is the scanning electron microscope (SEM) photograph with the coding microball in dopamine embodiment of the present invention before surface modification；
Fig. 6 is the scanning electron microscope (SEM) photograph with the coding microball in dopamine embodiment of the present invention after surface modification.
Specific embodiment
The present invention is further elaborated below against attached drawing and in conjunction with the embodiments:
The present invention provides a kind of preparation method of coding microball, in a specific embodiment, comprising the following steps:
(1) encoded material is mixed with aqueous oligomer, corresponding water-soluble photoinitiator dissolution is added completely, and vibrate and stir
It mixes uniformly, forms stable suspension as water phase；
(2) alkanes solvent and emulsifier mixing shaken well are formed into oily phase；
(3) water phase in step (1) is instilled in the oily phase in the step (2) in stirring, the oil phase
Volume is 20-30 times of the water phase volume, the suspension system of even suspension is continued stirring until after dripping, and to the suspension
System carries out ultraviolet light prolonged exposure；
(4) after being washed the product after solidification for several times, the microballoon of target grain size is screened, obtains institute after dry
State coding microball.
It in some preferred embodiments, can also be using the combination of one or more of following characteristics.
In the step (3), the wavelength of the ultraviolet light is 355-375nm, irradiation energy 200-250mW.
The encoded material includes fluorescence-encoded material and laser induced breakdown spectroscopy encoded material.
The fluorescence-encoded material is semiconductor fluorescence quantum dot；The laser induced breakdown spectroscopy encoded material is containing gold
Belong to the nano material of element.
Aqueous oligomer in the step (1) includes epoxy acrylic resin class (such as epoxy acrylate), polyurethane
Crylic acid resin (such as urethane acrylate), polyester acrylate resin class (such as polyester acrylate), acroleic acid esterification third
Olefin(e) acid resinae (such as acroleic acid esterification polyacrylic resin) and unsaturated polyester (UP) class；The aqueous initiator includes benzophenone
Class, thioxanthones, diaryl phosphin be oxide-based and 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone.
Aqueous oligomer in the step (1) is polyethyleneglycol diacrylate, and the water-soluble photoinitiator is 2- hydroxyl
Base -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone；In every milliliter of polyethyleneglycol diacrylate, 2- hydroxyl -4'- (2- hydroxyl second
Oxygroup) -2- methyl phenyl ketone content be 10-30 milligrams.
In the step (1), the alkanes solvent be hexadecane, the emulsifier be cetyl polyethylene glycol, described ten
The volume of six alkane is 15-25 times of the volume of the cetyl polyethylene glycol.
In the step (3), the speed of stirring is 500-700 revolutions per minute, and the time persistently stirred is 1-2 minutes,
The time of the ultraviolet light prolonged exposure is 10-20 minutes.
In the step (4), washed using hexamethylene and alcohol mixed solution；The volume of the hexamethylene and ethyl alcohol
Than for 2:1-1:2.
In the step (4), the microballoon of target grain size is screened using stainless steel tm screen, the stainless steel micron
The size of sieve is -500 mesh of 400 mesh.
Below by way of two more specific embodiments, the present invention is further elaborated.
Embodiment 1
The CdSe/ZnS quantum dot of 100 microlitres of water solubility 520nm is mixed with 1 milliliter of polyethyleneglycol diacrylate, is added
Enter 20 milligrams of photoinitiator 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone dissolutions completely, and vibrates and stir evenly, shape
At stable suspension as water phase；20 milliliters of hexadecanes are taken, 1 milliliter of emulsifier cetyl polyethylene glycol is added, mixing oscillation is equal
The oily phase of even formation；By in oily mutually merging small beaker, it is put into magneton, according to 600 rpms of progress magnetic agitations, water phase is inhaled
Pipe instills in the oily phase in stirring, and after being added dropwise to complete, persistently stirring 1 minute, (wavelength is to ultraviolet lamp is opened after even suspension
355-375nm, energy 200mW) it is placed in above small beaker, prolonged exposure, curing time continues 10 minutes；After taking out solidification
For several times, remaining solid is suspended in ethyl alcohol using hexamethylene and ethyl alcohol mixing washing lotion (V/V, 1:1) centrifuge washing for suspension,
The target grain size of -450 mesh of 400 mesh is screened using stainless steel tm screen, is placed in vacuum oven, 40 DEG C of dryings obtain for 24 hours
To 525nm fluorescence spectrum coding microball.The scanning electron microscope (SEM) photograph of coding microball obtained in this example and under the microscope figure difference
As depicted in figs. 1 and 2；Fig. 3 is the decoding spectrum of coding microball obtained in this example.
For the quantum dot of the quantum dot of other materials or other wavelength of fluorescence (such as other single wavelengths or multiple wavelength)
Coding microball can be prepared using method made above, the coding microball that the additional amount of quantum dot obtains as needed
Attribute can be determined routinely.
Embodiment 2
10 milligrams of zinc oxide nano-particles are mixed with 1 milliliter of polyethyleneglycol diacrylate, 20 milligrams of addition is light-initiated
The dissolution of agent 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone completely, and is vibrated and is stirred evenly, and is formed stable suspension and is made
For water phase；20 milliliters of hexadecanes are taken, 1 milliliter of emulsifier cetyl polyethylene glycol is added, mixing shaken well forms oily phase；It will be oily
Mutually in merging small beaker, it is put into magneton, according to 700 rpms of progress magnetic agitations, water phase suction pipe is instilled in stirring
Oily phase persistently stirs 2 minutes and is placed in small burning to opening ultraviolet lamp (wavelength 355-375nm, energy 250mW) after even suspension
Cup top, prolonged exposure, curing time continue 20 minutes；The suspension after solidifying is taken out, is washed using hexamethylene and ethyl alcohol mixing
For several times, remaining solid is suspended in ethyl alcohol for liquid (V/V, 1:1) centrifuge washing, using stainless steel tm screen by -450 mesh of 400 mesh
Target grain size screen, be placed in vacuum oven, 40 DEG C of dryings obtain the laser-induced breakdown comprising zinc atom spectrum for 24 hours
Optical spectrum encoded microballoon.The laser induced breakdown spectroscopy decoding spectrum of coding microball obtained is as shown in Figure 4 in this example.
The nano material that other are contained with metallic element (such as magnesia) can also be obtained corresponding using method made above
Coding microball.
The good hydrophilic property of coding microball in embodiment of the present invention, it is in an experiment, hydrophily coding of the invention is micro-
It ball (if can be coding microball made from embodiment 1, being also possible to coding microball obtained etc. in embodiment 2) and existing dredges
Aqueous polystyrene microsphere is individually dispersed in two centrifuge tubes equipped with water, observes its dispersion feelings in water respectively
Condition, the coding microball in embodiment of the present invention can be suspended in water with stable dispersion, wall not easy to stick, and hydrophobic polystyrene
Wall then can be assembled, agglomerate and glue in water to microballoon.Coding microball in embodiment of the present invention (such as can be embodiment 1 to make
Coding microball, be also possible to coding microball obtained etc. in embodiment 2) carry out dopamine surface modification, such as Fig. 5 and Fig. 6
Shown, Fig. 5 is the scanning electron microscope (SEM) photograph of the coding microball of dopamine before surface modification, and Fig. 6 is the coding of dopamine after surface modification
The scanning electron microscope (SEM) photograph of microballoon, it can be seen from the figure that the surface of coding microball in the present embodiment is to be easy to carry out table
Face modification.
Claims (10)
1. a kind of preparation method of coding microball, it is characterised in that: the following steps are included:
(1) encoded material is mixed with aqueous oligomer, corresponding water-soluble photoinitiator dissolution is added completely, and it is equal to vibrate stirring
It is even, stable suspension is formed as water phase；
(2) alkanes solvent and emulsifier mixing shaken well are formed into oily phase；
(3) water phase in step (1) is instilled in the oily phase in the step (2) in stirring, the volume of the oil phase
It is 20-30 times of the water phase volume, the suspension system of even suspension is continued stirring until after dripping, and to the suspension system
Carry out ultraviolet light prolonged exposure；The ultraviolet light prolonged exposure includes being irradiated above the suspension system with ultraviolet lamp；
(4) after being washed the product after solidification for several times, the microballoon of target grain size is screened, obtains the volume after dry
Code microballoon.
2. preparation method according to claim 1, it is characterised in that: in the step (3), the wavelength of the ultraviolet light is
355-375nm, irradiation energy 200-250mW.
3. preparation method according to claim 1, it is characterised in that: the encoded material includes fluorescence-encoded material and swashs
Photoinduction breakdown spectral encoded material.
4. preparation method according to claim 3, it is characterised in that: the fluorescence-encoded material is semiconductor fluorescence quantum
Point；The laser induced breakdown spectroscopy encoded material is the nano material containing metallic element.
5. preparation method according to claim 1, it is characterised in that: the aqueous oligomer in the step (1) includes ring
Oxypropylene acid resin class, polyurethane acrylic resin class, polyester acrylate resin class, acrylated acrylics class and not
Saturated polyester class；The aqueous initiator includes that benzophenone, thioxanthones, diaryl phosphin be oxide-based and 2- hydroxyl-
4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone.
6. the preparation method according to claim 4, it is characterised in that: the aqueous oligomer in the step (1) is poly- second
Omega-diol diacrylate, the water-soluble photoinitiator are 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone；Every milliliter poly-
In glycol diacrylate, the content of 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone is 10-30 milligrams.
7. preparation method according to claim 1, it is characterised in that: in the step (1), the alkanes solvent is 16
Alkane, the emulsifier are cetyl polyethylene glycol, and the volume of the hexadecane is the 15- of the volume of the cetyl polyethylene glycol
25 times.
8. preparation method according to claim 1, it is characterised in that: in the step (3), the speed of stirring is 500-
700 revolutions per minute, the time persistently stirred are 1-2 minutes, and the time of the ultraviolet light prolonged exposure is 10-20 minutes.
9. preparation method according to claim 1, it is characterised in that: mixed using hexamethylene and ethyl alcohol in the step (4)
Solution is closed to be washed；The volume ratio of the hexamethylene and ethyl alcohol is 2:1-1:2.
10. preparation method according to claim 1, it is characterised in that: in the step (4), using stainless steel tm screen
The microballoon of target grain size is screened, the size of the stainless steel tm screen is -500 mesh of 400 mesh.
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