CN105713126A - Plasma preparation method of polystyrene fluorescent microspheres and reaction equipment of plasma preparation method - Google Patents
Plasma preparation method of polystyrene fluorescent microspheres and reaction equipment of plasma preparation method Download PDFInfo
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- CN105713126A CN105713126A CN201610067024.8A CN201610067024A CN105713126A CN 105713126 A CN105713126 A CN 105713126A CN 201610067024 A CN201610067024 A CN 201610067024A CN 105713126 A CN105713126 A CN 105713126A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/52—Polymerisation initiated by wave energy or particle radiation by electric discharge, e.g. voltolisation
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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- C09K2211/1003—Carbocyclic compounds
- C09K2211/1007—Non-condensed systems
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1014—Carbocyclic compounds bridged by heteroatoms, e.g. N, P, Si or B
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/182—Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide
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Abstract
The invention discloses a plasma preparation method of polystyrene fluorescent microspheres and reaction equipment of the plasma preparation method, and relates to the technical field of organic synthesis of fluorescent microspheres. A rare earth organic complex is adopted as a starting raw material, plasma of polystyrene is polymerized on the surface of the rare earth organic complex to coat the surface of the rare earth organic complex with a layer of polystyrene, and thus polystyrene fluorescent microspheres are formed. The method includes the main steps of 1, performing plasma pretreatment of the rare earth organic complex; 2, performing plasma polymerization, wherein plasma of polystyrene monomers is polymerized and deposited on the surface of the rare earth organic complex. The polystyrene fluorescent microspheres obtained through the preparation method have a long fluorescent lifetime and good heat stability, and the preparation process is simple, easy to perform and free of environmental pollution.
Description
Technical field
The present invention relates to fluorescent microsphere technical field of organic synthesis.
Background technology
Polymer fluorescent microspheres refer to diameter nanometer and micron order between, and be loaded with the polymer microballoon of fluorescent material, its shape is generally spherical.Wherein, fluorescent microsphere, with its stable morphosis and stable and efficient luminous efficiency, has huge application potential in labelling, intelligence analysis, detection, immobilized enzyme, the immunity field such as medical science, high-flux medicaments sifting.Therefore, the concern of domestic and international researcher is in recent years increasingly received about the research of high performance polymer fluorescent microspheres, it has also become the focus of this area research and difficult point.Polymer fluorescent microspheres containing rare earth organic complex had both had the high efficiency light-emitting characteristic of metal organic complex, the advantages such as the toughness and the machinability that contain again polymer microballoon, increasingly mature along with technology of preparing and means of testing, it has also become the key areas of functional microsphere material science research.Mechanical Behavior of Polystyrene is good, and heat stability is high, and becomes and prepare the carrier material that microsphere is conventional.
The preparation method of polymer fluorescent microspheres is broadly divided into two kinds: i.e. physical method and chemical method.And physical method is divided into investment, absorption method and self-assembly method；Chemical method is then divided into Graft Method and copolymerization method.The main deficiency that said method exists is that step is various, complex technical process, and most use organic solvent, and not only cost is high, and environmental pollution is heavier, brings inconvenience to practical application.Therefore, the simple new method of polymer fluorescent microspheres is prepared in exploration has become the new problem of Chinese scholars joint research.
Summary of the invention
The technical problem to be solved is to provide plasma preparation method and the consersion unit thereof of a kind of polystyrene fluorescent microsphere, obtained polystyrene fluorescent microsphere fluorescence lifetime is long, and properties of product are stable, and preparation process is simple, easy to implement, it does not have environmental pollution.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the plasma preparation method of a kind of polystyrene fluorescent microsphere, employing rare earth organic complex is initiation material, by cinnamic plasma polymerization on rare earth organic complex surface, wrap up a strata styrene, form polystyrene fluorescent microsphere；The key step of described preparation method includes:
1) the plasma pretreatment of rare earth organic complex；
2) plasma polymerization: make styrene monomer plasma polymerization and be deposited on rare earth organic complex surface.
Preferably, plasma polymerization is: plasma polymerization discharge parameter condition is pressure 8～20Pa, plasma pulse width to be 20～100s, plasma polymerization power be 45～125W, plasma polymerization time are 60～250min, reaction temperature is 60～90 DEG C.
Preferably, the molecular structural formula of rare earth organic complex is:
Preferably, the plasma pretreatment mode of rare earth organic complex is: 1～5g rare earth organic complex is joined in the quartzy bottle of the indoor rotation of plasma polymerization, gas to the air pressure extracting plasma polymerization indoor is 2Pa, then passing into high pure nitrogen to air pressure to plasma polymerization room is 80Pa, repeat extraction gas three times, regulating plasma polymerization room pressure is 20Pa, when discharge power 60W, by nitrogen gas plasma, rare earth organic complex is processed 15 minutes.
Preferably, quartz bottle rotary speed is 60～120rpm.
Preferably, plasma polymerizing step is: by raw material monomer bottle to the styrene monomer passing into gasification in plasma polymerization room, adjusts reaction room pressure；Make pulse radio-frequency power supply, adjusts plasma polymerization discharge parameter condition, starts electric discharge, after reaching the required plasma polymerization time, closes pulse radiation frequency power supply, stops electric discharge, continues to pass into the styrene monomer of gasification, and keeps 1.5 hours with this understanding.
A kind of consersion unit used by plasma preparation method of polystyrene fluorescent microsphere, including plasma polymerization room, relatively it is provided with anelectrode and negative electrode, anelectrode and negative electrode above and below plasma polymerization outside respectively to be connected with pulse radiation frequency power supply；Plasma polymerization room sidewall is provided with driving motor, and chamber, plasma polymerization indoor is provided with the quartzy bottle placed of laying across, and quartz bottle bottleneck is connected with driving motor, is provided with heater one, is provided with cellular through hole in the middle part of at the bottom of quartz bottle bottle outside quartz bottle；Plasma polymerization room is connected with gas suction device, gas supply device and vacuometer.
Preferably, gas suction device includes vacuum pump, and vacuum pump is connected with plasma polymerization room by vacuum-pumping pipeline.
Preferably, gas supply device includes raw material monomer bottle and nitrogen gas cylinder, and raw material monomer bottle is connected with plasma polymerization room by gas feed line with nitrogen gas cylinder；Raw material monomer bottle is connected with heater two.
Preferably, heater one is for adding hot jacket or heating wire.
Adopt and have the beneficial effects that produced by technique scheme: the polystyrene fluorescent microsphere obtained by this preparation method has longer fluorescence lifetime and good heat stability, and preparation process is simple, easy to implement, it does not have environmental pollution, embody the new concept of design of material.
Accompanying drawing explanation
Fig. 1 is the consersion unit structural representation of the present invention；
In figure, 1, nitrogen gas cylinder；2, heater two；3, raw material monomer bottle；4, gas feed line；5, driving motor；6, negative electrode；7, heater one；8, quartz bottle；9, cellular through hole；10, plasma polymerization room；11, pulse radiation frequency power supply；12, plasma polymerization room door；13, vacuometer；14, anelectrode；15, vacuum pump；16, vacuum-pumping pipeline.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
As it is shown in figure 1, consersion unit of the present invention includes plasma polymerization room 10, being relatively provided with anelectrode 14 and negative electrode 6 above and below outside plasma polymerization room 10 respectively, anelectrode 14 is connected with pulse radiation frequency power supply 11 with negative electrode 6；Plasma polymerization room 10 sidewall is provided with driving motor 5, plasma polymerization room 10 inner chamber is provided with the quartzy bottle 8 placed of laying across, quartz bottle 8 bottleneck is connected with driving motor 5, is provided with heater 1, is provided with cellular through hole 9 in the middle part of at the bottom of 8 bottles of bottle of quartz outside quartz bottle 8；Plasma polymerization room 10 is connected with gas suction device, gas supply device and vacuometer 13.
Gas suction device includes vacuum pump 15, and vacuum pump 15 is connected with plasma polymerization room 10 by vacuum-pumping pipeline 16.Gas supply device includes raw material monomer bottle 3 and nitrogen gas cylinder 1, and raw material monomer bottle 3 is connected with plasma polymerization room 10 by gas feed line 4 with nitrogen gas cylinder 1；Raw material monomer bottle 3 is connected with heater 22.Heater 1 is for adding hot jacket or heating wire.
Embodiment 1
A kind of plasma preparation method of polystyrene fluorescent microsphere, wherein:
The molecular structural formula of rare earth organic complex is:
Main preparation process includes:
(1) the plasma pretreatment of rare earth organic complex:
1g rare earth organic complex is joined in the quartzy bottle 8 of the rotation in plasma polymerization room 10, gas to the air pressure extracted in plasma polymerization room 10 is 2Pa, then passing into high pure nitrogen to air pressure to plasma polymerization room 10 is 80Pa, repeat extraction gas three times, regulating pressure in plasma polymerization room 10 is 20Pa, when discharge power 60W, by nitrogen gas plasma, rare earth organic complex is processed 15 minutes.
(2) plasma polymerization, styrene monomer plasma polymerization is also deposited on rare earth organic complex surface: rise to 60 DEG C by the temperature in heater one 7 quartz bottle 8, the rotary speed of quartz bottle 8 is adjusted to 60rpm, then passing through raw material monomer bottle 3 and pass into the styrene monomer of gasification in plasma polymerization room 10, adjusting reaction room pressure is 8Pa；Make pulse radio-frequency power supply 11, adjusts plasma polymerization discharge parameter condition, and plasma pulse width is 20s, plasma polymerization power is 125W, starts electric discharge, and the plasma polymerization time closes pulse radiation frequency power supply 11 after reaching 60min, stops electric discharge；Continue to pass into the styrene monomer of gasification, and keep 1.5 hours with this understanding, obtain polystyrene fluorescent microsphere.
Embodiment 2 embodiment 7
It is different in that from embodiment 1 plasma polymerization discharge parameter condition is different, including the temperature in plasma polymerization room pressure, quartz bottle, quartz bottle rotary speed, plasma pulse width, plasma polymerization power and plasma polymerization time, each embodiment plasma polymerization actual conditions is in Table 1.
The performance test results of the polystyrene fluorescent microsphere that embodiment 1～7 prepares is in Table 2.
Polystyrene fluorescent microsphere obtained by preparation method of the present invention has longer fluorescence lifetime and good heat stability, and preparation process is simple, it is easy to implements, it does not have environmental pollution, embodies the new concept of design of material.
Claims (10)
1. the plasma preparation method of a polystyrene fluorescent microsphere, it is characterized in that: employing rare earth organic complex is initiation material, by cinnamic plasma polymerization on rare earth organic complex surface, wrap up a strata styrene, form polystyrene fluorescent microsphere；The key step of described preparation method includes:
1) the plasma pretreatment of rare earth organic complex；
2) plasma polymerization: make styrene monomer plasma polymerization and be deposited on rare earth organic complex surface.
2. the plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 1, it is characterised in that described plasma polymerization is: plasma polymerization discharge parameter condition is pressure 8～20Pa, plasma pulse width to be 20～100s, plasma polymerization power be 45～125W, plasma polymerization time are 60～250min, reaction temperature is 60～90 DEG C.
3. the plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 1, it is characterised in that the molecular structural formula of described rare earth organic complex is:
。
4. the plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 1, it is characterized in that: the plasma pretreatment mode of rare earth organic complex is: 1～5g rare earth organic complex is joined in the quartzy bottle (8) of the rotation in plasma polymerization room (10), gas to the air pressure extracted in plasma polymerization room (10) is 2Pa, then passing into high pure nitrogen to air pressure to plasma polymerization room (10) is 80Pa, repeat extraction gas three times, regulating plasma polymerization room (10) interior pressure is 20Pa, when discharge power 60W, by nitrogen gas plasma, rare earth organic complex is processed 15 minutes.
5. the plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 4, it is characterised in that: quartz bottle (8) rotary speed is 60～120rpm.
6. the plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 1, it is characterized in that, plasma polymerizing step is: by raw material monomer bottle (3) to the styrene monomer passing into gasification in plasma polymerization room (10), adjusts reaction room pressure；Make pulse radio-frequency power supply (11), adjusts plasma polymerization discharge parameter condition, starts electric discharge, after reaching the required plasma polymerization time, close pulse radiation frequency power supply (11), stop electric discharge, continue to pass into the styrene monomer of gasification, and keep 1.5 hours with this understanding.
7. the consersion unit used by plasma preparation method of a kind of polystyrene fluorescent microsphere as claimed in claim 1, it is characterized in that: include plasma polymerization room (10), plasma polymerization room (10) is provided with anelectrode (14) and negative electrode (6) above and below outside respectively relatively, and anelectrode (14) is connected with pulse radiation frequency power supply (11) with negative electrode (6)；Plasma polymerization room (10) sidewall is provided with driving motor (5), plasma polymerization room (10) inner chamber is provided with the quartzy bottle (8) placed of laying across, quartz bottle (8) bottleneck is connected with driving motor (5), quartz bottle (8) outside is provided with heater one (7), is provided with cellular through hole (9) in the middle part of at the bottom of quartz bottle (8) bottle；Plasma polymerization room (10) is connected with gas suction device, gas supply device and vacuometer (13).
8. the consersion unit used by plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 7, it is characterized in that: gas suction device includes vacuum pump (15), and vacuum pump (15) is connected with plasma polymerization room (10) by vacuum-pumping pipeline (16).
9. the consersion unit used by plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 7, it is characterized in that: gas supply device includes raw material monomer bottle (3) and nitrogen gas cylinder (1), and raw material monomer bottle (3) is connected with plasma polymerization room (10) by gas feed line (4) with nitrogen gas cylinder (1)；Raw material monomer bottle (3) is connected with heater two (2).
10. the consersion unit used by plasma preparation method of a kind of polystyrene fluorescent microsphere according to claim 7, it is characterised in that: heater one (7) is for adding hot jacket or heating wire.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105482014A (en) * | 2016-01-29 | 2016-04-13 | 河北科技大学 | Preparation method of PMMA-based azo photosensitive microspheres and reaction equipment of preparation method |
| WO2018124205A1 (en) * | 2016-12-28 | 2018-07-05 | 片山化学工業株式会社 | Phosphorus-containing (meth)acrylate ester derivative |
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| CN103469174A (en) * | 2013-09-18 | 2013-12-25 | 河北科技大学 | Preparation method of cyanate ester resin thin film as well as reaction equipment thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105482014A (en) * | 2016-01-29 | 2016-04-13 | 河北科技大学 | Preparation method of PMMA-based azo photosensitive microspheres and reaction equipment of preparation method |
| CN105482014B (en) * | 2016-01-29 | 2017-07-07 | 河北科技大学 | The preparation method and its consersion unit of a kind of photosensitive microballoon of PMMA bases azo |
| WO2018124205A1 (en) * | 2016-12-28 | 2018-07-05 | 片山化学工業株式会社 | Phosphorus-containing (meth)acrylate ester derivative |
| CN110121501A (en) * | 2016-12-28 | 2019-08-13 | 片山化学工业株式会社 | Phosphorous (methyl) acrylate derivative |
| JPWO2018124205A1 (en) * | 2016-12-28 | 2019-10-31 | 片山化学工業株式会社 | Phosphorus-containing (meth) acrylic acid ester derivatives |
| CN110121501B (en) * | 2016-12-28 | 2023-04-04 | 片山化学工业株式会社 | Phosphorus-containing (meth) acrylate derivatives |
| JP7462913B2 (en) | 2016-12-28 | 2024-04-08 | 片山化学工業株式会社 | Phosphorus-containing (meth)acrylic acid ester derivatives |
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