CN106929007A - A kind of cyanic colours fluorescent material and preparation method thereof - Google Patents
A kind of cyanic colours fluorescent material and preparation method thereof Download PDFInfo
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- CN106929007A CN106929007A CN201710142879.7A CN201710142879A CN106929007A CN 106929007 A CN106929007 A CN 106929007A CN 201710142879 A CN201710142879 A CN 201710142879A CN 106929007 A CN106929007 A CN 106929007A
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- fluorescent material
- cadmium
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- cyanic colours
- colours fluorescent
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 239000003086 colorant Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 17
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- AGHQMAQBLOTWPQ-UHFFFAOYSA-H cadmium sulfate hydrate Chemical compound O.O.O.O.O.O.O.O.[Cd+2].[Cd+2].[Cd+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O AGHQMAQBLOTWPQ-UHFFFAOYSA-H 0.000 claims abstract description 4
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 239000011591 potassium Substances 0.000 claims abstract description 4
- WJFDCFHWFHCLIW-UHFFFAOYSA-N 2-(bromomethyl)-6-methylpyridine Chemical compound CC1=CC=CC(CBr)=N1 WJFDCFHWFHCLIW-UHFFFAOYSA-N 0.000 claims abstract description 3
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims description 11
- 239000011541 reaction mixture Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- OPGJGRWULGFTOS-UHFFFAOYSA-N 5-nitro-2,4-dioxo-1h-pyrimidine-6-carboxylic acid Chemical class OC(=O)C=1NC(=O)NC(=O)C=1[N+]([O-])=O OPGJGRWULGFTOS-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 150000005041 phenanthrolines Chemical class 0.000 abstract 1
- 239000013522 chelant Substances 0.000 description 4
- IFOZXUMSHBVSMA-UHFFFAOYSA-N 5-nitro-2,4-dioxo-1h-pyrimidine-6-carboxylic acid;potassium Chemical compound [K].OC(=O)C=1NC(=O)NC(=O)C=1[N+]([O-])=O IFOZXUMSHBVSMA-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000005725 8-Hydroxyquinoline Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002262 Schiff base Substances 0.000 description 1
- 150000004753 Schiff bases Chemical class 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000009994 optical bleaching Methods 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 229960003540 oxyquinoline Drugs 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/08—Cadmium compounds
-
- 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
- C09K2211/188—Metal complexes of other metals not provided for in one of the previous groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
Abstract
The invention discloses a kind of cyanic colours fluorescent material and preparation method thereof, the fluorescent material is the cadmium complex with certain space structure, its skeleton symbol:[Cd(C4N3O5)(C12H8N2)(H2O)]n;Its chemical formula is:CdC16H10N5O6, crystallographic system is monocline, and space group is C2/m, brilliant bag parameter α=90 °, β=107.10 °, γ=90 °, cadmium ion uses the coordination mode of seven coordination configurations.The preparation method of the fluorescent material compound is that, by Cadmium sulfate hydrate, 1, the mixture such as 10 phenanthrolines and 5 nitroorotic acid potassium and distilled water is placed in stainless steel cauldron, and cadmium complex has been obtained by hydro-thermal reaction.The preparation method is simple to operate, with low cost, is adapted to large-scale production.Obtained cadmium complex of the invention has good cyanic colours fluorescent emission performance, has potential application prospect as fluorescent material.
Description
Technical field
The invention belongs to the technical field of luminescent material, specifically on a kind of cyanic colours fluorescent material and its preparation side
Method.
Background technology
Since earlier 1900s, the research and application of fluorescent material are developed rapidly, especially organic fluorescence material
Material is widely used in weaving coloring, coloring plastic and printing color.Fluorescent material refer to material in the case where external light source is irradiated,
So as to obtain energy, generation is excited and causes luminous phenomenon.Ultraviolet radioactive, visible ray and infra-red radiation can cause fluorescent material
It is luminous.Fluorescent material has multiple use, and street road sign, building doorplate label, fire protection safety sign, billboard can be made with it
Deng.Fluorescent material is widely used in dyestuff, photooxidant, Optical Bleaching Agent, chemistry and the numerous areas such as bioanalysis, it
Materia medica, physiology, environmental science, information science technology aspect all have broad application prospects.
Organic fluorescence materials generally have can absorb the group or structure of exciting light, typically be conjugated bond structure, such as:Conjugation
π keys, benzene ring structure or similar benzene ring structure.Some organic ligands are luminous weaker in itself, and strong hair is become after forming metal complex
Stimulative substance, such as 8-hydroxyquinoline hardly light in itself, but the 8-hydroxyquinoline aluminum complex for being formed has hair well
Optical property, is the star molecule in luminescent substance.Some presence of Schiff-base complex also have good luminescent properties (Hamada Y etc.
J.Appl.Phys.,1996,35,L1339).With increasingly deep, the new metal organic complexes that people are studied fluorescent material
Thing is continued to bring out as fluorescent material.Nitroorotic acid complex has few quantifier elimination to report as fluorescent material, such as Hu Xiufeng
Et al. report a kind of purple fluorescence material and preparation method thereof, grant number CN102329610B;Li Xing, Bing Yue et al. are reported
The cadmium of purple luminescence property-nitroorotic acid compound (CrystEngComm, 2011,13,6373).The present invention discloses a kind of tool
There is the cadmium complex of specific composition and space structure, the complex has stronger fluorescent emission in the case where 330nm excites light action, most
Big emission peak 470nm, it has potential application prospect as fluorescent material.
The content of the invention
The technical problem to be solved in the present invention is directed to prior art, there is provided one kind has good cyanic colours emanative glimmering
Luminescent material and preparation method thereof.
The technical scheme taken regarding to the issue above of the present invention is:A kind of cyanic colours fluorescent material, the cyanic colours fluorescence
Material is the cadmium complex with certain space structure, its skeleton symbol:[Cd(C4N3O5)(C12H8N2)(H2O)]n, its chemical formula
For:CdC16H10N5O6, crystallographic system is monocline, and space group is C2/m, brilliant bag parameter
α=90 °, β=107.10 °, γ=90 °, cadmium ion uses the coordination mode of seven coordination configurations.
The preparation method of above-mentioned cyanic colours fluorescent material, comprises the following steps:
(1) a certain amount of Cadmium sulfate hydrate (CdSO is weighed4·H2O), a certain amount of 5- nitroorotic acids potassium and 1,10- are luxuriant and rich with fragrance
Sieve quinoline, is placed in the polytetrafluoroethyllining lining of 25mL stainless steel cauldrons, plus 10~distilled water of 15mL, stirs 20~30min,
Obtain reaction mixture solution, Cd (II) in reaction mixture solution:5- nitroorotic acid roots:Ratio=1 of the amount of substance of phenanthroline
~1.5:1:1;
(2) it is placed in air dry oven after stainless steel cauldron of the sealing equipped with above-mentioned reaction mixture solution, 120~
160 DEG C are reacted 48~72 hours, and reaction end is cooled to room temperature, are opened reactor and are obtained colourless acicular crystal;
(3) colourless acicular crystal is taken out, with absolute ethanol washing, is dried, that is, obtain described cyanic colours fluorescent material.
Preferably, the material for participating in reaction is that chemistry is pure.
Compared with prior art, the method have the characteristics that:
With Cadmium sulfate hydrate, 5- nitroorotic acids potassium and 1,10- phenanthroline for raw material carries out hydro-thermal reaction in autoclave,
The carboxyl of 5- nitroorotic acids is sloughed and in-situ oxidation is into carbonyl (- C=O) during the course of the reaction, the N at carbonyl and part ortho position
One Cd (II) ion of chelant, forms quaternary chelant ring, and one-dimensional chain structure (Fig. 1) is expanded into by chelant, and the structure has firm
Property conjugate property, is conducive to electron transition and energy transmission, so that compound has good optical activity.The hydro-thermal reaction
Synthesize a kind of new cadmium complex, the complex has accurate space structure and accurate molecular formula, used as a kind of ultramarine
Color luminescent material has a good application prospect.
Brief description of the drawings
Fig. 1 is the coordination context diagram of metal ion in cyanic colours fluorescent material cadmium complex of the invention;
Fig. 2 is the fluorescence emission spectrum of cyanic colours fluorescent material cadmium complex of the invention.
Specific embodiment
The present invention is further told about in detail below in conjunction with accompanying drawing embodiment.
Embodiment 1:
Weigh the CdSO of 0.0226g (0.1mmol)4·H2The 5- nitroorotic acid potassium list water of O, 0.0257g (0.1mmol)
Compound, hydration 1, a 10- phenanthrolines of 0.0198 (0.1mmol), is placed in the polytetrafluoroethyllining lining of 25mL stainless steel cauldrons
In, plus 10mL distilled water, stir 20min, obtain reaction mixture solution;Sealing is stainless equipped with above-mentioned reaction mixture solution
It is placed in air dry oven after steel reactor, 120 DEG C are reacted 48 hours, reaction end is cooled to room temperature, opens reactor and obtain nothing
Color acicular crystal;Colourless acicular crystal is taken out, with absolute ethanol washing, is dried, that is, obtained cyanic colours fluorescent material cadmium and coordinate
Thing.
Embodiment 2:
Weigh the CdSO of 0.0339g (0.15mmol)4·H2The 5- nitroorotic acid potassium list water of O, 0.0257g (0.1mmol)
Compound, hydration 1, a 10- phenanthrolines of 0.0198 (0.1mmol), is placed in the polytetrafluoroethyllining lining of 25mL stainless steel cauldrons
In, plus 15mL distilled water, stir 30min, obtain reaction mixture solution;Sealing is stainless equipped with above-mentioned reaction mixture solution
It is placed in air dry oven after steel reactor, 160 DEG C are reacted 72 hours, reaction end is cooled to room temperature, opens reactor and obtain nothing
Color acicular crystal;Colourless acicular crystal is taken out, with absolute ethanol washing, is dried, that is, obtained cyanic colours fluorescent material cadmium and coordinate
Thing.
Embodiment 3:
Weigh the CdSO of 0.0339g (0.15mmol)4·H2The 5- nitroorotic acid potassium lists of O, 0.0308g (0.12mmol)
Hydrate, hydration 1, a 10- phenanthrolines of 0.0238 (0.12mmol), is placed in the polytetrafluoroethylene (PTFE) of 25mL stainless steel cauldrons
In lining, plus 15mL distilled water, stir 25min, obtain reaction mixture solution;Sealing is equipped with above-mentioned reaction mixture solution not
It is placed in air dry oven after rust steel reactor, 150 DEG C are reacted 60 hours, reaction end is cooled to room temperature, opens reactor and obtain
Colourless acicular crystal;Colourless acicular crystal is taken out, with absolute ethanol washing, is dried, that is, obtained cyanic colours fluorescent material cadmium and match somebody with somebody
Compound.
Cyanic colours fluorescent material cadmium complex obtained in above-described embodiment is colourless acicular crystal, and its chemical formula is:
CdC16H10N5O6, its skeleton symbol is:[Cd(C4N3O5)(C12H8N2)(H2O)]n;The 5- nitroorotic acids decarboxylation in hydro-thermal reaction
Oxidation and chelant schematic diagram are as follows:
The coordination context diagram of metal ion is as shown in Figure 1 (for illustrative clarity, hydrogen in cyanic colours fluorescent material cadmium complex
Atom is omitted, and symmetry operation atom out is not marked).
Fluorescence property test is carried out after resulting cyanic colours fluorescent material cadmium complex is air-dried, in 330nm exciting lights
The lower cadmium complex of effect has stronger fluorescent emission, maximum emission peak 470nm, it is shown that good cyanic colours fluorescent emission
Can, its fluorescence spectrum is as shown in Figure 2.
Claims (3)
1. a kind of cyanic colours fluorescent material, it is characterised in that the fluorescent material is the cadmium complex with certain space structure, its
Skeleton symbol:[Cd(C4N3O5)(C12H8N2)(H2O)]n;Its chemical formula is:CdC16H10N5O6, crystallographic system is monocline, and space group is
C2/m, brilliant bag parameter α=90 °, β=107.10 °, γ=90 °, cadmium ion is adopted
With the coordination mode of seven coordination configurations.
2. a kind of preparation method of cyanic colours fluorescent material as claimed in claim 1, it is characterised in that comprise the following steps:
(1) a certain amount of Cadmium sulfate hydrate (CdSO is weighed4·H2O), a certain amount of 5- nitroorotic acids potassium and 1,10- phenanthroline,
It is placed in the polytetrafluoroethyllining lining of 25mL stainless steel cauldrons, plus 10~distilled water of 15mL, stir 20~30min, obtains instead
Mixture solution is answered, Cd (II) in reaction mixture solution:5- nitroorotic acid roots:Ratio=1 of the amount of substance of phenanthroline~
1.5:1:1;
(2) it is placed in air dry oven after stainless steel cauldron of the sealing equipped with above-mentioned reaction mixture solution, 120~160 DEG C
Reaction 48~72 hours, reaction end is cooled to room temperature, opens reactor and obtains colourless acicular crystal;
(3) colourless acicular crystal is taken out, with absolute ethanol washing, is dried, that is, obtain described cyanic colours fluorescent material.
3. the preparation method of cyanic colours fluorescent material according to claim 2, it is characterised in that the thing of the participation reaction
Matter is pure for chemistry.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108440581A (en) * | 2018-05-08 | 2018-08-24 | 宁波大学 | A kind of 5- nitroorotic acids mononuclear zinc complex and its preparation method and application |
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