CN106750357A - A kind of rare earth polymer green fluorescent material and preparation method thereof - Google Patents
A kind of rare earth polymer green fluorescent material and preparation method thereof Download PDFInfo
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- CN106750357A CN106750357A CN201710019896.1A CN201710019896A CN106750357A CN 106750357 A CN106750357 A CN 106750357A CN 201710019896 A CN201710019896 A CN 201710019896A CN 106750357 A CN106750357 A CN 106750357A
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 27
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 18
- 229920000642 polymer Polymers 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 108010043121 Green Fluorescent Proteins Proteins 0.000 title claims abstract description 9
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims abstract description 22
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 22
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims abstract description 20
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 238000012916 structural analysis Methods 0.000 claims description 3
- 238000012790 confirmation Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 230000009967 tasteless effect Effects 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- -1 rare earth ion Chemical class 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000021615 conjugation Effects 0.000 description 2
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000012718 coordination polymerization Methods 0.000 description 1
- 238000009510 drug design Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- 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
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- 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
- 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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- 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
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Luminescent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a kind of rare earth polymer green fluorescent material and preparation method thereof.A kind of rare earth polymer green fluorescent material chemical name is that the Phen of three glutaric acid two closes two terbiums, chemical formula：[Tb2(C12H8N2)2(C5H6O4)3]n；Structural formula is[Tb2(C12H8N2)2(C5H6O4)3]nIt is the crystal grown by hydrothermal synthesis method.Preparation method is with glutaric acid, Phen and TbCl3For raw material obtains product by hydrothermal synthesis method.Advantages of the present invention：Preparation method of the present invention has the advantages that process is simple, efficient, cheap, pollution-free, reproducible.The advantage of the material is that heat endurance is good and luminous intensity is strong.
Description
Technical field
The invention belongs to fluorescent material technical field.Specifically a kind of rare earth polymer green fluorescent material and its preparation side
Method.
Background technology
Phosphor material powder was come out in 1938 earliest, and early stage Stokes et al. has synthesized the fluorescent material such as artificial schellite and for glimmering
In light lamp.Phosphate phosphor is have developed again in people in 1948, and this light-emitting phosphor performance is than early stage light-emitting phosphor
Can have and significantly improve.60~seventies of 20th century fluorescent material be widely used.Studied not with to fluorescent material
It is disconnected to go deep into, it has been developed that three primary colors fluorescent powder, introduces in fluorescent material using rare earth element as activator, it is the hair of fluorescent material
Optical property is significantly improved.Fluorescent material mainly has sulfide-based fluorescent material, aluminate-series fluorescent material, phosphoric acid in the market
Salt system fluorescent material, fluorescent RE powder etc..
Rare earth element ion is due to its special electron structure and abundant energy level so that it turns into mankind's luminescent material
Treasure-house.Because the f-f transition of rare earth ion belongs to forbidden transition, therefore very weak suction is shown in visible ray and ultraviolet region
Receive so that single rare earth ion it is luminous relatively weak, but when rare earth ion and organic ligand cooperation obtain complex when, due to
Organic ligand usually has larger absorption in ultra-violet (UV) band, and by effective Intramolecular energy transfer, by its excitation state
Energy transmission, so as to be greatly promoted the characteristic emission of rare earth ion, strengthens its luminous effect to the emission level of rare earth ion
Should.Rare earth coordination polymer fluorescent material is to pass through the special chemical combination that is self-assembly of by rare earth metal cations and organic ligand
Thing, it has the crystal structure similar to Inorganic crystal compound, but its synthesis has Modulatory character, therefore can be by topology
The rational design of structure and the Expanding design of organo-functional group synthesize the coordination polymerization with particular characteristic.By to it is organic into
Divide and rare earth ion is scientifically and rationally screened and regulated and controled, the size of control metal ion and conjugation primitive, it is possible to achieve right
The regulation and control of emission wavelength.On the other hand, by the design to molecular material, can study specific between molecular structure and performance
Relation, explores the luminescence mechanism of material, so as to provide foundation to design new and effective fluorescent material.Based on this viewpoint, we
A kind of rare earth polymer fluorescent material [Tb with green luminescence property is synthesized using hydro-thermal method2(C12H8N2)2(C5H6O4)3]n,
Test shows that the compound has preferable heat endurance and fluorescence property.
The content of the invention
It is an object of the invention to provide a kind of rare earth polymer green fluorescent material and preparation method thereof.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
1. a kind of rare earth polymer green fluorescent material
1) chemical name is that the Phen of three glutaric acid two closes two terbiums；
Chemical formula：[Tb2(C12H8N2)2(C5H6O4)3]n。
2) structural formula is
3) physicochemical property：Outward appearance is brown rhabdolith, and tasteless is insoluble in organic solvent and water.
2. the Phen of three glutaric acid two closes the preparation method of two terbiums, and concrete operations are as follows：Glutaric acid is weighed respectively
0.0264g (0.2mmol), Phen 0.0270g (0.15mmol), TbCl3It is anti-that 0.0743g (0.28mmol) is added to 20ml
Answer in kettle, add 2ml distilled water, be uniformly mixed, instill triethylamine regulation pH=5~6, install reactor, be positioned over
7 days in 100 DEG C of insulating boxs, take out reactor and be allowed to naturally cool to room temperature, suction filtration, and with distilling water washing, air drying, i.e.,
For the Phen of three glutaric acid two closes two terbiums.
3. the Phen of three glutaric acid of compound two closes the confirmation of two terbiums, and 3 penta are confirmed using APEXII CCD diffractometers
The Phen of diacid two closes two terbiums：The rare earth polymer crystal that will be prepared is in Bruke smart APEXII CCD diffractometers
On, with Mo K α (λ=0.071073nm) ray of graphite monochromator monochromatization, scanned in ω-θ modes.Under 296K, receive altogether
Collection point diffraction.Through complete matrix least square method to F2It is modified the completion of structural analysis SHELXL-97 software kits.Compound
Molecular formula is C39H34N4O12Tb2, relative molecular weight is 1068.56g/mol, and crystal is anorthic system, and space group is P-1, structure cell
Parameter is α=83.909 (2) °,
β=84.340 (2) °, γ=74.984 (2) °,Z=2.
4. compound structure analysis
The rare earth polymer fluorescent material [Tb2(C12H8N2)2(C5H6O4)3]nDisplaying two-dimensional layered structure, Tb3+Ion with
Glutaric acid is connected with each other, and forms two-dimensional layer.Phen plays structural modification effect, further with Tb3+Complex cation is chelated.It is dilute
Contain optically active Tb in native polymer3+With the big π keys of conjugation in Phen molecule, electron transition and energy is conducive to pass
Pass, cause the rare earth polymer that there is good green fluorescence performance.
5. purposes
Optical performance test shows that rare earth polymer has good green fluorescence performance (545nm), and luminous intensity is suitable
By force, it is contemplated that have significant application value in fields such as color monitor, fluorescence labeling, Fluorescent falsification-preventing fiber, fluorescent paints.
Advantages of the present invention：
Rare earth polymer fluorescent material [the Tb that the present invention is provided2(C12H8N2)2(C5H6O4)3]nIt is by hydrothermal synthesis method
The crystal for growing.Preparation method of the present invention has process is simple, efficient, cheap, pollution-free, reproducible etc. excellent
Point.The advantage of the material is that heat endurance is good and luminous intensity is strong.
Brief description of the drawings
Fig. 1 is a kind of fluorescence spectra of rare earth polymer green fluorescent material of the invention.
In figure：Ordinate is fluorescence intensity, and abscissa is wavelength of fluorescence.
Specific embodiment
With reference to embodiment, the invention will be further described.
1. the Phen of three glutaric acid two closes the preparation of two terbiums
Embodiment 1
The Phen of three glutaric acid two closes the preparation of two terbiums
Glutaric acid 0.0264g (0.2mmol), Phen 0.0270g (0.15mmol), TbCl are weighed respectively3
0.0743g (0.28mmol) is added in 20ml reactors, adds 2ml distilled water, is uniformly mixed, and is instilled triethylamine and is adjusted
Section pH is 5, installs reactor, is positioned over 7 days in 100 degrees Celsius of insulating boxs, takes out reactor and is allowed to naturally cool to room temperature, is gone out
Existing bulk crystals.Take out crystal prototype distillation water washing, air drying.Yield 83% is (with TbCl3It is standard).
Embodiment 2
The Phen of three glutaric acid two closes the preparation of two terbiums
Glutaric acid 0.0264g (0.2mmol), Phen 0.0270g (0.15mmol), TbCl are weighed respectively30.0743g
(0.28mmol) is added in 20ml reactors, adds 2ml distilled water, is uniformly mixed, and is instilled triethylamine regulation pH and is
6, reactor is installed, it is positioned over 7 days in 100 degrees Celsius of insulating boxs, take out reactor and be allowed to naturally cool to room temperature, occur block
Crystal.Take out crystal prototype distillation water washing, air drying.Yield 83% is (with TbCl3It is standard).
The rare earth coordination polymer crystal that will be prepared uses graphite monochromatic on Bruke smart APEXII CCD diffractometers
Mo K α (λ=0.071073nm) ray of device monochromatization, is scanned in ω-θ modes.Under 296K, point diffraction is collected altogether.Through complete
Matrix least square method is to F2It is modified the completion of structural analysis SHELXL-97 software kits.The molecular formula of compound is
C39H34N4O12Tb2, relative molecular weight is 1068.56g/mol, and crystal is anorthic system, and space group is P-1, and cell parameter is α=83.909 (2) °, β=84.340
(2) °, γ=74.984 (2) °, Z=2.
2. the Phen of three glutaric acid two closes the performance test of two terbiums
Tested by XRF and shown, the polymer has green fluorescence at 545nm, and functional, such as Fig. 1 institutes
Show.
Claims (3)
1. a kind of rare earth polymer green fluorescent material, it is characterised in that
1) chemical name is that the Phen of three glutaric acid two closes two terbiums；
Chemical formula：[Tb2(C12H8N2)2(C5H6O4)3]n；
2) structural formula is
3) physicochemical property：Outward appearance is brown rhabdolith, and tasteless is insoluble in organic solvent and water.
2. the Phen of three glutaric acid two as claimed in claim 1 closes the preparation method of two terbiums, it is characterised in that specific behaviour
Make as follows：Glutaric acid 0.0264g i.e. 0.2mmol is weighed respectively, and Phen 0.0270g is 0.15mmol, TbCl30.0743g
That is 0.28mmol is added in 20ml reactors, adds 2ml distilled water, is uniformly mixed, and instills triethylamine regulation pH=5
~6, reactor is installed, it is positioned over 7 days in 100 DEG C of insulating boxs, take out reactor and be allowed to naturally cool to room temperature, suction filtration is used in combination
Distillation water washing, air drying, the as Phen of three glutaric acid two close two terbiums.
3. the Phen of three glutaric acid of compound two closes the confirmation of two terbiums, it is characterised in that utilize APEXII CCD diffractometers
Confirm that the Phen of three glutaric acid two closes two terbiums：The rare earth polymer crystal that will be prepared is in Bruke smart APEXII CCD
On diffractometer, with Mo K α (λ=0.071073nm) ray of graphite monochromator monochromatization, scanned in ω-θ modes.In 296K
Under, point diffraction is collected altogether；Through complete matrix least square method to F2It is modified the completion of structural analysis SHELXL-97 software kits；
The molecular formula of compound is C39H34N4O12Tb2,Relative molecular weight is 1068.56g/mol, and crystal is anorthic system, and space group is
P-1, cell parameter isα=83.909
(2) °, β=84.340 (2) °, γ=74.984 (2) °,Z=2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876820A (en) * | 2019-03-13 | 2019-06-14 | 重庆师范大学 | A kind of 17 water two protonation hydration boron vanadic acid nickel potassium and its preparation with photocatalysis performance |
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2017
- 2017-01-11 CN CN201710019896.1A patent/CN106750357B/en not_active Expired - Fee Related
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| CN1560060A (en) * | 2004-03-01 | 2005-01-05 | 南开大学 | Synthesis for compound of diamine bridge linking ortho phenanthroline hydrous lanthanum (III) and anti-cancer activity thereof |
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| CN109876820A (en) * | 2019-03-13 | 2019-06-14 | 重庆师范大学 | A kind of 17 water two protonation hydration boron vanadic acid nickel potassium and its preparation with photocatalysis performance |
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