CN104673272A - Broadband fluorescent material and preparation method thereof - Google Patents
Broadband fluorescent material and preparation method thereof Download PDFInfo
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- CN104673272A CN104673272A CN201310634289.8A CN201310634289A CN104673272A CN 104673272 A CN104673272 A CN 104673272A CN 201310634289 A CN201310634289 A CN 201310634289A CN 104673272 A CN104673272 A CN 104673272A
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- fluorescent material
- broadband
- sulphadiazine sodium
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- cpds
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Abstract
The invention discloses a broadband fluorescent material and a preparation method thereof. Sulfadiazine with conjugated pai bond and 2,2'-dipyridine chemically react with optically active zinc ions to prepare the sulfadiazine zinc compound with certain space structure, wherein the molecular formula is C30H26N10O4S2Zn, and the molecular weight is 720.10. The crystal system is triclinic, the space group is P-1, and the cell parameters are as follows: a=10.3593A, b=12.5083A, c=12.6513A, alpha=75.5403 degrees, beta=74.4553 degrees, and gamma=83.0593 degrees. The zinc ion is in a geometrical configuration of a distorted octahedron, and the bond lengths are respectively 0.2044nm, 0.2086nm, 02130nm, 0.2168nm, 0.2243nm and 0.2581nm. The compound fluorescent material has strong fluorescence emission within the range of 380-480nm under the excitation of 267nm light, and has wide application prospects when be used as a fluorescent material.
Description
Technical field
The invention belongs to technical field of material chemistry, be specifically related to a kind of broadband fluorescent material and preparation method thereof.
Background technology
Fluorescence is exactly from the adjoint luminescence phenomenon of the radiative transition process of lowest excited singlet state, and the rate constant of luminescence process is large, and the life-span of excited state is short.Have the material of fluorescent both, its molecule often has following characteristics: (1) has large conjugated double bond (π key) system; (2) there is the two dimensional structure of rigidity; (3) substituting group on ring is to electron substituent group group; (4) its minimum electron excitation singlet state is (π, π *) type.Along with the progress of science and technology, the research of people to fluorescence gets more and more, and the range of application of fluorescent substance is more and more wider.Fluorescent substance, except being used as dyestuff, also obtaining in fields such as pigment dyestuff, optical whitening agent, photooxidant, coating, chemistry and biochemical analysis, sun power trap, anti-fake mark, pharmaceutical indications and laser and applies widely.
Fluorescent material to be coordinated with trace active agent by metal (zinc, chromium) sulfide or rare earth oxide to form through calcining.Colourless or shallow white, is under UV-light (200 ~ 400nm) is irradiated, according to the difference of metal in pigment and activator species, content, and presents the visible ray (400 ~ 800nm) of shades of colour.Fluorescent material roughly can be divided into following three classes by material structure: the aromatic fused ring compound with rigid structure, the Intramolecular charge transfer with conjugated structure and some a metal-organic complex, the Intramolecular charge transfer wherein with conjugated structure is the class studying the most extensive and active at present, and is the luminophor that a class has good radiative decay ability.This is because this type of material is when its absorb light is excited and is in excited state, in molecule, original charge density distribution there occurs change, there occurs photoinduced charge transfer in molecule, cause molecular polarization, its charge density distribution is made mainly to concentrate on the two ends of molecule, thus photoisomerization reaction is less likely to occur, therefore becoming a class has compound compared with high-fluorescence quantum yield.
As far back as 1575, the yellow aqueous solution just having people to observe lignum nephriticum section in the sun presented very lovely sky blue.1852, G.G. when stokes observes quinine and chlorophyll solution with spectrometer, find that the wavelength of the wavelength ratio incident light of the light that they send is slightly long, distinguish that this phenomenon is luminous energy again send the light of different wave length due to material absorbing thus, instead of cause due to light diffusion effect.Stokes claims this light to be fluorescence.Along with day by day deep to fluorescence Quality Research, new fluorescent material continues to bring out, it has a wide range of applications in multiple field.
Recent study finds: have optically active metal ion and demonstrate good luminescent properties with the metal organic micromolecule compound assembled containing the organic ligand of conjugation primitive.Such research comprises: organic composition and inorganic components can carry out autotelic screening to the size of metal ion or conjugation primitive, thus emission wavelength regulation; In addition, on a molecular scale, can the synthesis of designing material, be conducive to research material relation be-tween structure and properties like this and explore its luminescence mechanism, thus providing theoretical foundation for design advanced luminescent material.Being allocated by organic composition and inorganic components is prepare one of broadband fluorescent material effective way.Broadband fluorescent material refers under certain excitation, has a class material of fluorescent emission in relative broad range.The advantage of broadband fluorescent material has high fluorescent and luminosity, has high luminous efficiency, applied range etc.The present invention is with zinc salt, Sulphadiazine Sodium and 2, and 2 '-dipyridyl is raw material, and prepared a kind of novel Sulphadiazine Sodium zn cpds, this compound has potential application prospect as a kind of broadband fluorescent material.
Summary of the invention
Technical problem to be solved by this invention is for prior art, provides a kind of and has broadband fluorescent material of good fluorescent emission performance and preparation method thereof.
The present invention is the technical scheme taked that solves the problem: a kind of broadband fluorescent material, this fluorescent material is a kind of Sulphadiazine Sodium zn cpds with certain space structure, and its molecular formula is C
30h
26n
10o
4s
2zn, crystallographic system is three tiltedly, and spacer is P-1, unit cell parameters a=10.3593
b=12.5083
c=12.6513
α=75.5403 °, β=74.4553 °, γ=83.0593 °, zine ion is the octahedral geometric configuration of distortion, and bond distance is respectively: 0.2044nm, 0.2086nm, 02130nm, 0.2168nm, 0.2243nm and 0.2581nm.Wherein bond distance 0.2581nm is long especially, and not within normal range, it plays a part the delicate of complexity to the energy level variations of zine ion, makes this compound have unique fluorescent emission performance.Under 267nm optical excitation, described Sulphadiazine Sodium zn cpds all demonstrates stronger fluorescent emission from 380nm to 480nm in scope, is a kind of fluorescent emission broadband fluorescent material of good performance.
Preferably, the structural unit of described broadband fluorescent material is:
The preparation method of above-mentioned Sulphadiazine Sodium zn cpds broadband fluorescent material, comprises the following steps:
(1) take zinc salt, Sulphadiazine Sodium and 2 that mol ratio is 5:4 ~ 6:4 ~ 6:4 ~ 6,2 '-dipyridyl and KOH are placed in glass reaction bottle;
(2) add ethanol and the deionized water of volume ratio 1:2 ~ 4, microwave back flow reaction 10 ~ 30 minutes, then put into stainless steel cauldron and seal, in 60 ~ 100 DEG C of heating 36 ~ 60h;
(3), after reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
Preferably, the described material participating in reaction is chemical pure.
Preferably, the described zinc salt participating in reaction is zinc nitrate, zinc acetate or zinc sulfate.
Compared with prior art, the invention has the advantages that: with compound zinc salt, Sulphadiazine Sodium and 2,2 '-dipyridyl is that raw material carries out microwave and solvent thermal reaction, obtained a kind of new Sulphadiazine Sodium zn cpds, this compound, as fluorescent material, has space structure (Fig. 1) and accurately molecular formula accurately; Containing enriching optically active Zn (II) ion, pyridine atom N and the large π key of conjugation etc. in molecule, be conducive to transition of electron and transmission ofenergy, in addition, the energy level of coordinate bond to zine ion grown especially plays delicate regulating effect, thus makes compound have unique photoelectric activity.Under 267nm optical excitation, described Sulphadiazine Sodium zn cpds all demonstrates stronger fluorescent emission from 380nm to 480nm in scope, is a kind of fluorescent emission broadband fluorescent material of good performance, has a wide range of applications as fluorescent material.
Accompanying drawing explanation
Fig. 1 is the structural unit figure of broadband fluorescent material of the present invention;
Fig. 2 is the fluorescence emission spectrum of broadband fluorescent material of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1:
Take Zn (NO
3)
26H
2o (60mg, 0.20mmol), Sulphadiazine Sodium (40mg, 0.16mmol), 2,2 '-dipyridyl (25mg, 0.16mmol) and KOH (9mg, 0.16mmol) are placed in 25mL glass reaction bottle, add 3.0mL ethanol and 6.0mL deionized water, microwave back flow reaction, after 10 minutes, proceeds in stainless steel cauldron and seals, at 60 DEG C of heating 60h.After reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
Embodiment 2:
Take Zn (OAc)
22H
2o (87mg, 0.40mmol), Sulphadiazine Sodium (80mg, 0.32mmol), 2,2 '-dipyridyl (50mg, 0.32mmol) and KOH (18mg, 0.32mmol) are placed in 25mL glass reaction bottle, add 3.0mL ethanol and 9.0mL deionized water, microwave back flow reaction, after 20 minutes, proceeds in stainless steel cauldron and seals, at 80 DEG C of heating 60h.After reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
Embodiment 3:
Take ZnSO
47H
2o (115mg, 0.40mmol), Sulphadiazine Sodium (100mg, 0.40mmol), 2,2 '-dipyridyl (62mg, 0.40mmol) and KOH (22mg, 0.40mmol) are placed in 25mL glass reaction bottle, add 3.0mL ethanol and 9.0mL deionized water, microwave back flow reaction, after 20 minutes, proceeds in stainless steel cauldron and seals, at 100 DEG C of heating 36h.After reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
Embodiment 4:
Take Zn (NO
3)
26H
2o (50mg, 0.20mmol), Sulphadiazine Sodium (60mg, 0.24mmol), 2,2 '-dipyridyl (37mg, 0.24mmol) and KOH (13mg, 0.24mmol) are placed in 25mL glass reaction bottle, add 3.0mL ethanol and 12.0mL deionized water, microwave back flow reaction, after 30 minutes, proceeds in stainless steel cauldron and seals, at 80 DEG C of heating 48h.After reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
The fluorescent material prepared in above-described embodiment after measured its molecular formula is C
30h
26n
10o
4s
2zn, its space structure figure as shown in Figure 1.
Carry out fluorescence property test by after obtained fluorescent material natural air drying, this compound demonstrates unique royal purple fluorescent emission performance.As shown in Figure 2.
Claims (5)
1. a broadband fluorescent material, is characterized in that, this fluorescent material is a kind of Sulphadiazine Sodium zn cpds with certain space structure, and its molecular formula is C
30h
26n
10o
4s
2zn, crystallographic system is three tiltedly, and spacer is P-1, unit cell parameters a=10.3593
b=12.5083
c=12.6513
α=75.5403 °, β=74.4553 °, γ=83.0593 °, zine ion is the octahedral coordination geometric configuration of distortion, and bond distance is respectively: 0.2044nm, 0.2086nm, 02130nm, 0.2168nm, 0.2243nm and 0.2581nm.Under 267nm optical excitation, described Sulphadiazine Sodium zn cpds all demonstrates stronger fluorescent emission from 380nm to 480nm in scope.
2. broadband fluorescent material according to claim 1, is characterized in that, the structural unit of described fluorescent material is:
3. a preparation method for broadband fluorescent material, is characterized in that, comprises the following steps:
Take zinc salt, Sulphadiazine Sodium and 2 that mol ratio is 5:4 ~ 6:4 ~ 6:4 ~ 6,2 '-dipyridyl and KOH are placed in glass reaction bottle;
Add ethanol and the deionized water of volume ratio 1:2 ~ 4, microwave back flow reaction 10 ~ 30 minutes, then put into stainless steel cauldron and seal, in 60 ~ 100 DEG C of heating 36 ~ 60h;
After reaction terminates, be cooled to room temperature, separate out colourless bulk crystals, be described fluorescent material.
4. preparation method according to claim 3, is characterized in that the described material participating in reaction is chemical pure.
5. a broadband fluorescent material, is characterized in that under 267nm optical excitation, and described Sulphadiazine Sodium zn cpds all demonstrates stronger fluorescent emission from 380nm to 480nm in relative broad range.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893582A (en) * | 2017-03-10 | 2017-06-27 | 宁波大学 | A kind of broadband fluorescent material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
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2013
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| ANGEL GARCı´A-RASO等: "Coordination behaviour of sulfanilamide derivatives.Crystal structures of [Hg(sulfamethoxypyridazinato)2],[Cd(sulfadimidinato)2(H2O)]P2H2O and [Zn(sulfamethoxazolato)2-(pyridine)2(H2O)2]", 《POLYHEDRON》, vol. 19, 3 March 2000 (2000-03-03), pages 991 - 1004 * |
| FANGFANG PAN等: "Switching from Bonding to Nonbonding: Temperature-Dependent Metal Coordination in a Zinc(II) Sulfadiazine Complex", 《INORG. CHEM.》, vol. 51, 22 December 2011 (2011-12-22), pages 769 - 771 * |
| 邴月: "氮杂环类金属超分子组装与性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, 15 March 2013 (2013-03-15), pages 014 - 145 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893582A (en) * | 2017-03-10 | 2017-06-27 | 宁波大学 | A kind of broadband 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 |
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Application publication date: 20150603 |