CN102329610A - Purple fluorescent material and a preparation method thereof - Google Patents
Purple fluorescent material and a preparation method thereof Download PDFInfo
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- CN102329610A CN102329610A CN201110285494A CN201110285494A CN102329610A CN 102329610 A CN102329610 A CN 102329610A CN 201110285494 A CN201110285494 A CN 201110285494A CN 201110285494 A CN201110285494 A CN 201110285494A CN 102329610 A CN102329610 A CN 102329610A
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- nitroorotic acid
- compound
- nitroorotic
- fluorescent material
- purple
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Abstract
The invention discloses a purple fluorescent material and a preparation method thereof. The preparation method comprises the following step: subjecting 5-nitroorotic acid with conjugate pi bonds and cadmium ions with optical activity to a chemical reaction to obtain a 5-nitroorotic acid cadmium compound with a certain spatial structure, wherein the molecular formula of the 5-nitroorotic acid cadmium compound is C18H21CdN5O9; a crystal system is monoclinic; a space group is P1/n; a cell parameter alpha is equal to 90.00 degrees; a cell parameter beta is equal to 99.967 degrees; a cell parameter gamma is equal to 90.00 degrees; the cadmium ions are in a tetragonal-pyramidal coordination mode; two nitrogen coordinating atoms are from pyridine propane; one nitrogen coordinating atom is from the 5-nitroorotic acid; one oxygen coordinating atom is from the 5-nitroorotic acid; and one oxygen coordinating atom is from coordinated water. The compound contains abundant optically active Cd (II) ions and the conjugate pi bonds; the electron transition and the energy transfer are beneficial, so that the compound has favorable photoelectric activity; and the prepared material has favorable purple fluorescence emission performance, and has a potential application foreground as a fluorescent material.
Description
Technical field
The invention belongs to the materials chemistry field, be specifically related to a kind of purple fluorescence material and preparation method thereof.
Background technology
The radiation that fluorescence is discharged when being the material low-energy state identical from the excited state inactivation to multiplicity.The most basic condition that compound can produce fluorescence is that its energy of being absorbed when the constant transition of multiplicity takes place is less than the most weak chemical bond energy needed of fracture.In the structure of compound, must have fluorophor as=C=O ,-N=O ,-N=N ,=C=N-,=C=S etc.When these groups were conjugated system a part of of molecule, then this compound possibly produce fluorescence.
Fluorescent material typically refers to after having accepted outside energy, can energy absorption be stored, and is converted into luminous energy in the place of dark.Be incorporated into the organic ligand that has optically active metals ion or contain the conjugation primitive in the fluorescent material, can greatly improve the luminescent properties of fluorescent material.The organic ligand that employing contains different conjugation primitives cooperates with metals ion, and sensitizing agent can be prepared the fluorescent material of various optical effects.
Fluorescent material is divided into organic fluorescence materials and inorganic fluorescent material.
Organic fluorescence materials can roughly be divided into following three types by material structure: (1) has the aromatic fused ring compound of rigid structure; (2) has the intramolecular charge transfer compounds of conjugated structure; (3) some a metal-organic complex.Wherein (2) class is one type that studies the most extensive and actively at present.(2) class has radiative decay ability preferably.This is because (2) type material is excited and when being in excited state when its absorb light; Variation has taken place in the original charge density distribution of intramolecularly; Intramolecularly photoinduction charge transfer has taken place; Cause that molecule intensifies, make its charge density distribution mainly concentrate on the two ends of molecule, thereby be not easy to take place the photoisomerization reaction.Therefore become one type of compound that higher Φ r value is arranged.Along with progress of science and technology, people are more and more to the research of fluorescence, and the range of application of fluorescent substance is more and more wider.After the sixties in last century, laser was found, under the effort of researcher, developed a large amount of fluorescent materials at home and abroad.Fluorescent material has obtained using widely in actual life.Fluorescent substance also is applied to fields such as pigment dyestuff, optical whitening agent, photooxidant, coating, chemistry and biochemical analysis, anti-fake mark, medicine spike and laser except that as the dyestuff.
Summary of the invention
Technical problem to be solved by this invention is to prior art, and a kind of purple fluorescence material with superperformance and preparation method thereof is provided.
The present invention solves the problems of the technologies described above the technical scheme of taking to be: a kind of purple fluorescence material, this fluorescent material are a kind of 5-nitroorotic acid cadmic compounds with certain space structure, and its molecular formula is C
18H
21CdN
5O
9, M=563.80.Crystallographic system is a monocline; Spacer is P2/n, unit cell parameters
α=90.00 °, β=99.967 °; γ=90.00 °; Cadmium ion is the tetragonal pyramid coordination mode, and 2 nitrogen ligating atoms come from pyridine propane, and 1 nitrogen ligating atom comes from the 5-nitroorotic acid; 1 oxygen ligating atom comes from the 5-nitroorotic acid, and 1 oxygen ligating atom comes from coordinated water.
1) in the 25mL tetrafluoroethylene with 1～2: respectively add 5-nitroorotic acid at 1～4: 1～3, Cd (Ac)
22H
2O, pyridine propane adds the water of 5～15ml then, stirs it is mixed.Tetrafluoroethylene is put into stainless steel cauldron.
2) baking oven is put in the reaction kettle sealing, 60～120 ℃ of heating 12-72h; Naturally cool to room temperature then, open reaction kettle and get clear crystal.
3) clear crystal that makes is washed natural air drying with mother liquor; Through measuring, the molecular formula of this cadmic compound is C
18H
21CdN
5O
9
Said 5-nitroorotic acid, Cd (Ac)
22H
2The mol ratio of O and pyridine propane is 1～2: 1～4: 1～3.
The temperature of said system reaction is 60～120 ℃, and the reaction times is 12-72h.
The material of said participation reaction is analytical pure.
Compared with prior art; The invention has the advantages that: will have conjugated the 5-nitroorotic acid and with have optically active cadmium ion and carry out chemical reaction and make novel nitroorotic acid cadmic compound, this compound has space structure (Fig. 1) and molecular formula accurately accurately as the purple fluorescence material; Contain and enrich optically active Cd (II) ion and conjugated, help transition of electron and transmission ofenergy, thereby make compound have good photoelectric activity.Prepared material has good purple fluorescence emitting performance, has the potential application prospect as fluorescent material.
Description of drawings
Fig. 1 is 5-nitroorotic acid cadmium structural unit figure of the present invention;
Fig. 2 is a 5-nitroorotic acid cadmium fluorescence emission spectrum of the present invention.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1:
Adding 5-nitroorotic acid in the 25mL polytetrafluoroethyllining lining (0.5mmol, 1.129g), Cd (Ac)
22H
2(0.5mmol, 0.134g), (0.5mmol 0.107g), adds an amount of water 5mL to pyridine propane to O, stirs it is mixed.Tetrafluoroethylene is put into stainless steel cauldron.
Baking oven is put in the reaction kettle sealing, 60 ℃ of heating 72h; Naturally cool to room temperature then, open reaction kettle and get clear crystal.
Embodiment 2:
Adding 5-nitroorotic acid in the 25mL polytetrafluoroethyllining lining (0.5mmol, 1.129g), Cd (Ac)
22H
2(1.0mmol, 0.268g), (1.5mmol 0.321g), adds an amount of water 10mL to pyridine propane to O, stirs it is mixed.Tetrafluoroethylene is put into stainless steel cauldron.
Baking oven is put in the reaction kettle sealing, 100 ℃ of heating 48h; Naturally cool to room temperature then, open reaction kettle and get clear crystal.
Embodiment 3:
Adding 5-nitroorotic acid in the 25mL polytetrafluoroethyllining lining (0.5mmol, 1.129g), Cd (Ac)
22H
2(2.0mmol, 0.536g), (1.0mmol 0214g), adds an amount of water 15mL to pyridine propane to O, stirs it is mixed.Tetrafluoroethylene is put into stainless steel cauldron.
Baking oven is put in the reaction kettle sealing, 120 ℃ of heating 12h; Naturally cool to room temperature then, open reaction kettle and get clear crystal.
The clear crystal that makes is washed natural air drying with mother liquor; Through measuring, the molecular formula of this cadmic compound is C
18H
21CdN
5O
9, crystallographic system is a monocline, spacer is P2/n, unit cell parameters
α=90.00 °, β=99.967 °, γ=90.00 °; Cadmium ion is the tetragonal pyramid coordination mode, and 2 nitrogen ligating atoms come from pyridine propane, and 1 nitrogen ligating atom comes from the 5-nitroorotic acid; 1 oxygen ligating atom comes from the 5-nitroorotic acid, and 1 oxygen ligating atom comes from coordinated water.Figure is as shown in Figure 1 for its crystalline structure.
With prepared cadmic compound C
18H
21CdN
5O
9Carry out the fluorescence property test, this compound exhibits goes out good purple emitting performance (like Fig. 2).
Claims (5)
1. a purple fluorescence material is characterized in that this fluorescent material is a kind of 5-nitroorotic acid cadmic compound with certain space structure, and its molecular formula is C
18H
21CdN
5O
9, crystallographic system is a monocline, spacer is P1/n, unit cell parameters
α=90.00 °, β=99.967 °, γ=90.00 °; Cadmium ion is the tetragonal pyramid coordination mode, and 2 nitrogen ligating atoms come from pyridine propane, and 1 nitrogen ligating atom comes from the 5-nitroorotic acid; 1 oxygen ligating atom comes from the 5-nitroorotic acid, and 1 oxygen ligating atom comes from coordinated water.
2. the described purple fluorescence preparation methods of claim 1 is characterized in that may further comprise the steps:
1) in the 25mL tetrafluoroethylene with 1～2: respectively add 5-nitroorotic acid at 1～4: 1～3, Cd (Ac)
22H
2O, pyridine propane adds the water of 5～15ml then, stirs it is mixed.Tetrafluoroethylene is put into stainless steel cauldron.
2) baking oven is put in the reaction kettle sealing, 60～120 ℃ of heating 12-72h; Naturally cool to room temperature then, open reaction kettle and get clear crystal.
3) clear crystal that makes is washed natural air drying with mother liquor; Through measuring, the molecular formula of this cadmic compound is C
18H
21CdN
5O
9
3. purple fluorescence preparation methods according to claim 2 is characterized in that said 5-nitroorotic acid, Cd (Ac)
22H
2The mol ratio of O and pyridine propane is 1～2: 1～4: 1～3.
4. purple fluorescence preparation methods according to claim 2 is characterized in that the temperature of said system reaction is 60～120 ℃, and the reaction times is 12-72h.
5. purple fluorescence preparation methods according to claim 2 is characterized in that the material of said participation reaction is analytical pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110285494 CN102329610B (en) | 2011-09-23 | 2011-09-23 | Purple fluorescent material and a preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110285494 CN102329610B (en) | 2011-09-23 | 2011-09-23 | Purple fluorescent material and a preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102329610A true CN102329610A (en) | 2012-01-25 |
| CN102329610B CN102329610B (en) | 2013-07-10 |
Family
ID=45481582
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|---|---|---|---|
| CN 201110285494 Expired - Fee Related CN102329610B (en) | 2011-09-23 | 2011-09-23 | Purple fluorescent material and a preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789212A (en) * | 2015-04-21 | 2015-07-22 | 徐伟鹏 | White light fluorescent powder for LED and preparation method thereof |
| CN106243136A (en) * | 2016-07-26 | 2016-12-21 | 宁波大学 | A kind of purple fluorescence material and preparation method thereof |
| CN106833624A (en) * | 2017-03-10 | 2017-06-13 | 宁波大学 | A kind of bluish violet fluorescent material and preparation method thereof |
| CN106893582A (en) * | 2017-03-10 | 2017-06-27 | 宁波大学 | A kind of broadband fluorescent material and preparation method thereof |
| CN106905246A (en) * | 2017-03-10 | 2017-06-30 | 宁波大学 | A kind of orange-yellow fluorescent material and preparation method thereof |
| CN106929007A (en) * | 2017-03-10 | 2017-07-07 | 宁波大学 | A kind of cyanic colours fluorescent material and preparation method thereof |
| CN106986899A (en) * | 2017-05-23 | 2017-07-28 | 宁波大学 | A kind of Imatinib super molecular compound and preparation method thereof |
| CN107266374A (en) * | 2017-06-12 | 2017-10-20 | 宁波大学 | A kind of monokaryon zinc super molecular complex and preparation method thereof |
| CN107325294A (en) * | 2017-06-12 | 2017-11-07 | 宁波大学 | A kind of nickel compound with porous two-dimensional layered structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008001101A2 (en) * | 2006-06-29 | 2008-01-03 | Astex Therapeutics Limited | Pharmaceutical combinations |
| CN102127426A (en) * | 2011-01-11 | 2011-07-20 | 宁波大学 | Fluorescent material with purple luminescence property and preparation method thereof |
-
2011
- 2011-09-23 CN CN 201110285494 patent/CN102329610B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008001101A2 (en) * | 2006-06-29 | 2008-01-03 | Astex Therapeutics Limited | Pharmaceutical combinations |
| CN102127426A (en) * | 2011-01-11 | 2011-07-20 | 宁波大学 | Fluorescent material with purple luminescence property and preparation method thereof |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789212A (en) * | 2015-04-21 | 2015-07-22 | 徐伟鹏 | White light fluorescent powder for LED and preparation method thereof |
| CN106243136A (en) * | 2016-07-26 | 2016-12-21 | 宁波大学 | A kind of purple fluorescence material and preparation method thereof |
| CN106243136B (en) * | 2016-07-26 | 2018-06-15 | 宁波大学 | A kind of purple fluorescence material and preparation method thereof |
| CN106893582A (en) * | 2017-03-10 | 2017-06-27 | 宁波大学 | A kind of broadband fluorescent material and preparation method thereof |
| CN106905246A (en) * | 2017-03-10 | 2017-06-30 | 宁波大学 | A kind of orange-yellow fluorescent material and preparation method thereof |
| CN106929007A (en) * | 2017-03-10 | 2017-07-07 | 宁波大学 | A kind of cyanic colours fluorescent material and preparation method thereof |
| CN106833624A (en) * | 2017-03-10 | 2017-06-13 | 宁波大学 | A kind of bluish violet fluorescent material and preparation method thereof |
| CN106929007B (en) * | 2017-03-10 | 2019-01-22 | 宁波大学 | A kind of cyanic colours fluorescent material and preparation method thereof |
| CN106893582B (en) * | 2017-03-10 | 2019-03-15 | 宁波大学 | A kind of broadband fluorescent material and preparation method thereof |
| CN106905246B (en) * | 2017-03-10 | 2019-04-16 | 宁波大学 | A kind of orange-yellow fluorescent material and preparation method thereof |
| CN106986899A (en) * | 2017-05-23 | 2017-07-28 | 宁波大学 | A kind of Imatinib super molecular compound and preparation method thereof |
| CN107266374A (en) * | 2017-06-12 | 2017-10-20 | 宁波大学 | A kind of monokaryon zinc super molecular complex and preparation method thereof |
| CN107325294A (en) * | 2017-06-12 | 2017-11-07 | 宁波大学 | A kind of nickel compound with porous two-dimensional layered structure and preparation method thereof |
| CN107266374B (en) * | 2017-06-12 | 2019-06-04 | 宁波大学 | A kind of monokaryon zinc super molecular complex and preparation method thereof |
| CN107325294B (en) * | 2017-06-12 | 2020-02-18 | 宁波大学 | Nickel compound with porous two-dimensional layered structure and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN102329610B (en) | 2013-07-10 |
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