CN105733560B - A kind of red fluorescence material and preparation method thereof - Google Patents
A kind of red fluorescence material and preparation method thereof Download PDFInfo
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- CN105733560B CN105733560B CN201610159026.XA CN201610159026A CN105733560B CN 105733560 B CN105733560 B CN 105733560B CN 201610159026 A CN201610159026 A CN 201610159026A CN 105733560 B CN105733560 B CN 105733560B
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 24
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical class OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 claims abstract description 16
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 15
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 8
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- DNXDYHALMANNEJ-UHFFFAOYSA-N furan-2,3-dicarboxylic acid Chemical class OC(=O)C=1C=COC=1C(O)=O DNXDYHALMANNEJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 4
- 238000011835 investigation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012742 biochemical analysis Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012926 crystallographic analysis Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009994 optical bleaching Methods 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- -1 photooxidant Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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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- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
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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
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
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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
- C09K2211/181—Metal complexes of the alkali metals and alkaline earth metals
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- 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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- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of red fluorescence material and preparation method thereof, the entitled [Eu of the fluorescent material3K2(FDA)4(NO3)3(MeCN)2]n, the molecular formula of the fluorescent material is：C28H14N5O29Eu3K2, molecular weight 1418.55, the furandicarboxylic acids of FDA 2,5.Its preparation method is that 2,5 furandicarboxylic acids, europium nitrate and potassium nitrate are put into autoclave, then adds acetonitrile solution, is reacted under conditions of 120 DEG C and obtains bulk crystals.[Eu3K2(FDA)4(NO3)3(MeCN)2]nThe red fluorescence of 70000a.u. intensity is produced under 395nm incident light irradiation.Present invention process is simple, chemical constituent is easily controllable, reproducible and yield is high.
Description
Technical field
The present invention relates to fluorescent material preparation field, more particularly to a kind of red fluorescence material and preparation method thereof.
Background technology
Modern fluorescence material has turned into the backing material in the fields such as presentation of information, lighting source, photoelectric device, can make
Luminous printing ink, luminous paint, luminescent plastic, luminous printing paste, organic pigment, Optical Bleaching Agent, photooxidant, coating, chemistry
And the field such as biochemical analysis, solar energy trap, anti-fake mark, pharmaceutical indications and laser has obtained wider application.It is but existing
The problem of poor performance be present in some fluorescent materials, particularly red fluorescence material.
The content of the invention
Based on the problems of above-mentioned prior art, the present invention provides a kind of red fluorescence material and preparation method thereof,
The excellent functional material of rubescent color fluorescence property can be synthesized.
In order to solve the above technical problems, the present invention provides a kind of red fluorescence material, the fluorescent material is entitled：[Eu3K2
(FDA)4(NO3)3(MeCN)2]n, the material molecule formula is：C28H14N5O29Eu3K2, molecular weight 1418.55, FDA 2,5- furans
Mutter dioctyl phthalate, crystal structural data is shown in Table one, and related bond distance's bond angle is shown in Table two；[Eu3K2(FDA)4(NO3)3(MeCN)2]n
The red fluorescence of 70000a.u. intensity is produced under 395nm incident light irradiation；
Table one is：[Eu3K2(FDA)4(NO3)3(MeCN)2]nCrystallographic parameter
Table two is：[Eu3K2(FDA)4(NO3)3(MeCN)2]nBond distanceWith bond angle (°)
Symmetry codes: (i) -x+2, -y+1, -z+2； (ii) x, -y+1, z-1/2； (iii) -x+
2, y, -z+3/2； (iv) x, -y,z-1/2； (v) -x+3/2, y+1/2, -z+3/2； (vi) -x+3/2, y-1/
2, -z+3/2； (vii) -x+3/2, -y+1/2, -z+1； (viii) x,-y+1, z+1/2； (ix) x, -y, z+1/
2。
The embodiment of the present invention also provides a kind of preparation method of red fluorescence material, for preparing red of the present invention
Fluorescent material [Eu3K2(FDA)4(NO3)3(MeCN)2]n, comprise the following steps：
FDCA, potassium nitrate and europium nitrate are mixed, are then added in acetonitrile solution, 120 after stirring
Reaction obtains colourless bulk crystals, as red fluorescence material [Eu under conditions of DEG C3K2(FDA)4(NO3)3(MeCN)2]n；This is glimmering
Luminescent material can launch the red fluorescence of 70000a.u. intensity under the incident light irradiation of 395nm wavelength.
In above-mentioned preparation method, the dosage of each raw material is：
The parts by weight of 2,5- furandicarboxylic acids 0.156~0.312, the parts by weight of potassium nitrate 0.101~0.202, europium nitrate 0.446
~0.892 parts by weight, the parts by weight of acetonitrile solution 40~80；
The colourless bulk crystals obtained after being reacted after the stirring under conditions of 120 DEG C are：Stirring 10 minutes, Ran Houfang
In 120 DEG C of baking oven after static 48h, cooling obtains colourless bulk crystals.
Beneficial effects of the present invention are：Raw material is easy to get, and fluorescence property is excellent, can be prepared with solvent-thermal process mode, work
Skill is simple, chemical constituent is easily controllable, reproducible and yield is high.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is red fluorescence material [Eu provided in an embodiment of the present invention3K2(FDA)4(NO3)3(MeCN)2]nCrystal knot
Composition；
Fig. 2 is fluorescence spectra provided in an embodiment of the present invention.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, rather than whole embodiments.Based on embodiments of the invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to protection scope of the present invention.
The embodiment of the present invention provides a kind of fluorescent material of rubescent color, and the red fluorescence material is entitled：[Eu3K2(FDA)4
(NO3)3(MeCN)2]n, molecular formula is：C28H14N5O29Eu3K2, molecular weight 1418.55, FDA is FDCA, brilliant
Body structured data is shown in Table one, and related bond distance's bond angle is shown in Table two；The red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n
The red fluorescence of 70000a.u. intensity is produced under 395nm incident light irradiation；
[the Eu of table one3K2(FDA)4(NO3)3(MeCN)2]nCrystallographic parameter
[the Eu of table two3K2(FDA)4(NO3)3(MeCN)2]nBond distanceWith bond angle (°)
Symmetry codes:(i)-x+2,-y+1,-z+2；(ii)x,-y+1,z-1/2；(iii)-x+2,y,-z+3/2；
(iv)x,-y,z-1/2；(v)-x+3/2,y+1/2,-z+3/2；(vi)-x+3/2,y-1/2,-z+3/2；(vii)-x+3/2,-y+
1/2,-z+1；(viii)x,-y+1,z+1/2；(ix)x,-y,z+1/2.
Above-mentioned red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]nSynthesized using solvent thermal process, synthesis tool
Body step is：
By 0.156~0.312g 2,5- furandicarboxylic acids and 0.101~0.202g potassium nitrate, 0.446~0.892g
Europium nitrate mixing resulting mixture, add mixture in 50~100ml acetonitrile solutions, stir 10 minutes, be then placed on 120
DEG C baking oven in after static 48h, cooling obtains colourless bulk crystals i.e. [Eu3K2(FDA)4(NO3)3(MeCN)2]n；Pass through list
Brilliant diffractometer determines its structure.Material is subjected to fluorometric investigation, it can launch under the exciting of 395nm wavelength
70000a.u. the red fluorescence of intensity.
The red fluorescence material and preparation method of the present invention are described further with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
By 0.156g FDCA and 0.101g potassium nitrate, 0.446g europium nitrate mixing resulting mixture,
It is added in 50ml acetonitrile solutions, stirs 10 minutes, be then placed in 120 DEG C of baking oven after static 48h, cooling obtains colourless
Bulk crystals, as red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n。
Product is characterized using following instrument and method：1st, the crystalline substance that size is 0.27 × 0.26 × 0.24mm3 is selected
Body is used for ray crystallographic analysis, and single crystal diffraction data are collected on Rigaku SCX diffractometers, with graphite monochromator monochromatization
Mok alpha rays (), 3.1 °≤θ≤27.5 °.Gained compound belongs to monoclinic system, and space group is all C2/c,
Cell parameter is aboutα=90 °, β=112.05 °, γ=
90°.The crystal structure of the fluorescent material is shown in Fig. 1 (using Diamond Software on Drawing).
Embodiment 2
0.312g FDCA and 0.202g potassium nitrate, 0.892g europium nitrate are mixed, then added
Into 100ml acetonitrile solutions, stir 10 minutes, be then placed in 120 DEG C of baking oven after static 48h, cooling obtains colourless block
Shape crystal, as red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n。
To red fluorescence material [Eu made from above-described embodiment3K2(FDA)4(NO3)3(MeCN)2]nCarry out fluorometric investigation,
It produces the red fluorescence of 70000a.u. intensity under 395nm incident light irradiation, obtains fluorescent spectrum curve result such as Fig. 2
It is shown.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (3)
1. a kind of red fluorescence material, it is characterised in that the fluorescent material is entitled：[Eu3K2(FDA)4(NO3)3(MeCN)2]n,
The molecular formula of the material is：C28H14N5O29Eu3K2, molecular weight 1418.55, FDA is FDCA, crystal structure number
According to being shown in Table one, related bond distance's bond angle is shown in Table two；[Eu3K2(FDA)4(NO3)3(MeCN)2]nProduced under 395nm incident light irradiation
The red fluorescence of raw 70000a.u. intensity；
Table one is：[Eu3K2(FDA)4(NO3)3(MeCN)2]nCrystallographic parameter
Table two is：[Eu3K2(FDA)4(NO3)3(MeCN)2]nBond distanceWith bond angle (°)
Symmetry codes:(i)-x+2,-y+1,-z+2；(ii)x,-y+1,z-1/2；(iii)-x+2,y,-z+3/2；(iv)
x,-y,z-1/2；(v)-x+3/2,y+1/2,-z+3/2；(vi)-x+3/2,y-1/2,-z+3/2；(vii)-x+3/2,-y+1/
2,-z+1；(viii)x,-y+1,z+1/2；(ix)x,-y,z+1/2.
2. a kind of preparation method of red fluorescence material, it is characterised in that for preparing the red fluorescence material described in claim 1
Expect [Eu3K2(FDA)4(NO3)3(MeCN)2]n, comprise the following steps：
FDCA, potassium nitrate and europium nitrate are mixed, are then added in acetonitrile solution, at 120 DEG C after stirring
Under the conditions of reaction obtain colourless bulk crystals, as red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n；The phosphor
Material can launch the red fluorescence of 70000a.u. intensity under the incident light irradiation of 395nm wavelength.
A kind of 3. preparation method of red fluorescence material according to claim 2, it is characterised in that the use of each raw material
Measure and be：
The parts by weight of 2,5- furandicarboxylic acids 0.156~0.312, the parts by weight of potassium nitrate 0.101~0.202, europium nitrate 0.446~
0.892 parts by weight, the parts by weight of acetonitrile solution 40~80；
Reaction obtains colourless bulk crystals and is under conditions of 120 DEG C after the stirring：Stirring 10 minutes, is then placed on 120 DEG C
Baking oven in after static 48h, cooling obtains colourless bulk crystals.
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Families Citing this family (7)
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| CN106957649B (en) * | 2017-04-17 | 2019-05-28 | 北京石油化工学院 | A kind of fluorescent material of green light and preparation method thereof |
| CN106957328B (en) * | 2017-04-17 | 2019-02-26 | 北京石油化工学院 | A kind of fluorescent material and preparation method thereof to glow |
| CN108913125B (en) * | 2018-09-29 | 2021-04-06 | 北京石油化工学院 | Red fluorescent material and preparation method thereof |
| CN109111473B (en) * | 2018-10-18 | 2021-04-30 | 北京石油化工学院 | Red fluorescent inorganic-organic hybrid material and preparation method thereof |
| CN109053776B (en) * | 2018-10-18 | 2021-04-30 | 北京石油化工学院 | Green terbium-based fluorescent material and preparation method thereof |
| CN109053775B (en) * | 2018-10-18 | 2021-04-02 | 北京石油化工学院 | Red europium-based fluorescent material and preparation method thereof |
| CN109053774B (en) * | 2018-10-18 | 2021-04-30 | 北京石油化工学院 | Green fluorescent inorganic-organic hybrid material and preparation method thereof |
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| CN102757453A (en) * | 2012-07-16 | 2012-10-31 | 南开大学 | Multifunctional rare earth metal-organic framework and preparation method thereof |
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2016
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757453A (en) * | 2012-07-16 | 2012-10-31 | 南开大学 | Multifunctional rare earth metal-organic framework and preparation method thereof |
| CN105037303A (en) * | 2015-07-07 | 2015-11-11 | 天津工业大学 | Method for preparing 2,5-furandicarboxylic acid from 5-hydroxymethyl furfural |
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| A Bimetallic Lanthanide Metal–Organic Material as a Self-Calibrating Color-Gradient Luminescent Sensor;Jingmin Zhou et al.;《Adv. Mater.》;20151007;第27卷;7072-7077 * |
| Crystal structure and luminescence of complexes of Eu(III) and Tb(III) with furan-2,5-dicarboxylate;Sebastiaan Akerboom et al.;《Inorganica Chimica Acta》;20120201;第387卷;289-293 * |
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