CN105733560A - Red fluorescent material and method for preparing same - Google Patents
Red fluorescent material and method for preparing same Download PDFInfo
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- CN105733560A CN105733560A CN201610159026.XA CN201610159026A CN105733560A CN 105733560 A CN105733560 A CN 105733560A CN 201610159026 A CN201610159026 A CN 201610159026A CN 105733560 A CN105733560 A CN 105733560A
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title abstract description 8
- 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
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical group OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005286 illumination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical class [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 abstract 4
- 239000000203 mixture Substances 0.000 description 4
- 238000011835 investigation 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
- 230000005260 alpha ray 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
- 239000000470 constituent Substances 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
- 238000002156 mixing Methods 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
Classifications
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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
-
- 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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- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a red fluorescent material and a method for preparing the same.The red fluorescent material is named as [Eu3K2 (FDA) 4 (NO3) 3 (MeCN)2]n, a molecular formula of the red fluorescent material is C28H14N5O29Eu3K2, a molecular weight of the red fluorescent material is 1418.55, and the FDA represents 2, 5-furan terephthalic acid.The method includes arranging the 2, 5-furan terephthalic acid, europium nitrate and potassium nitrate in a high-pressure reaction kettle; adding acetonitrile solution into the high-pressure reaction kettle; carrying out reaction under the condition of the temperature of 120 DEG C to obtain bulk crystals.Red fluorescent light with the intensity of 70000 a.u.can be generated when the red fluorescent material [Eu3K2 (FDA) 4 (NO3) 3 (MeCN)2]n is illuminated by incident light with the length of 396 nm.The red fluorescent material and the method have the advantages of simple process, easiness in controlling chemical components, good repeatability and high yield.
Description
Technical field
The present invention relates to fluorescent material preparation field, particularly relate to a kind of red fluorescence material and preparation method thereof.
Background technology
Modern fluorescence material become information show, the backing material in the field such as 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 catcher, anti-fake mark, pharmaceutical indications and laser has obtained wider application.But it is existing
The problem that some fluorescent materials, particularly red fluorescence material exist poor performance.
Summary of the invention
Based on the problem existing for above-mentioned prior art, the present invention provides a kind of red fluorescence material and preparation method thereof,
The functional material that rubescent color fluorescence property is excellent can be synthesized.
For solving above-mentioned technical problem, the present invention provides a kind of red fluorescence material, and this fluorescent material is entitled: [Eu3K2
(FDA)4(NO3)3(MeCN)2]n, this material molecule formula is: C28H14N5O29Eu3K2, molecular weight is 1418.55, and FDA is 2,5-furan
Muttering dioctyl phthalate, crystal structural data is shown in Table one, and relevant bond distance's bond angle is shown in Table two；[Eu3K2(FDA)4(NO3)3(MeCN)2]n?
The incident illumination of 395nm irradiates the lower red fluorescence producing 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。
The embodiment of the present invention also provides for the preparation method of a kind of red fluorescence material, is used for preparing redness 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, is then added in acetonitrile solution, 120 after stirring
Under conditions of DEG C, reaction obtains colourless bulk crystals, is red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n；This is glimmering
Luminescent material can launch the red fluorescence of 70000a.u. intensity under the incident illumination of 395nm wavelength irradiates.
In above-mentioned preparation method, the consumption of described each raw material is:
2,5-furandicarboxylic acid 0.156～0.312 weight portion, potassium nitrate 0.101～0.202 weight portion, europium nitrate 0.446
～0.892 weight portion, acetonitrile solution 40～80 weight portion；
The colourless bulk crystals obtained after reaction under conditions of 120 DEG C after described stirring is: stirs 10 minutes, then puts
In the baking oven of 120 DEG C after static 48h, cooling obtains colourless bulk crystals.
The invention have the benefit that raw material is easy to get, fluorescence property is excellent, can prepare by solvent-thermal process mode, work
Skill is simple, chemical constituent is easily controllable, reproducible and yield is high.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, required use in embodiment being described below
Accompanying drawing be briefly described, it should be apparent that, below describe in accompanying drawing be only some embodiments of the present invention, for this
From the point of view of the those of ordinary skill in field, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings
Accompanying drawing.
Red fluorescence material [the Eu that Fig. 1 provides for the embodiment of the present invention3K2(FDA)4(NO3)3(MeCN)2]nCrystal knot
Composition；
The fluorescence spectrum figure that Fig. 2 provides for the embodiment of the present invention.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment
It is only a part of 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 not making creative work premise, broadly falls into protection scope of the present invention.
The embodiment of the present invention provides the fluorescent material of a kind of rubescent color, and this red fluorescence material is entitled: [Eu3K2(FDA)4
(NO3)3(MeCN)2]n, molecular formula is: C28H14N5O29Eu3K2, molecular weight is 1418.55, and FDA is FDCA, brilliant
Body structured data is shown in Table one, and relevant bond distance's bond angle is shown in Table two；This red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n?
The incident illumination of 395nm irradiates the lower red fluorescence producing 70000a.u. intensity；
Table one [Eu3K2(FDA)4(NO3)3(MeCN)2]nCrystallographic parameter
Table two [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.
Above-mentioned red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]nSolvent thermal process is utilized to synthesize, synthesis tool
Body step is:
By 2,5-furandicarboxylic acid and the potassium nitrate of 0.101～0.202g, 0.446～the 0.892g of 0.156～0.312g
Europium nitrate be mixed into mixture, add mixture in 50～100ml acetonitrile solutions, stir 10 minutes, be then placed on 120
DEG C baking oven in after static 48h, it is [Eu that cooling obtains colourless bulk crystals3K2(FDA)4(NO3)3(MeCN)2]n；By list
Brilliant diffractometer measures its structure.Material is carried out fluorometric investigation, and it is under the exciting of 395nm wavelength, can launch
70000a.u. the red fluorescence of intensity.
With specific embodiment, red fluorescence material and the preparation method of the present invention are described further below in conjunction with the accompanying drawings.
Embodiment 1
The FDCA of 0.156g and the europium nitrate of the potassium nitrate of 0.101g, 0.446g are mixed into mixture,
Joining in 50ml acetonitrile solution, stir 10 minutes, be then placed in the baking oven of 120 DEG C after static 48h, cooling obtains colourless
Bulk crystals, is red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n。
Use following instrument and method that product is characterized: 1, to select the crystalline substance of a size of 0.27 × 0.26 × 0.24mm3
Body is used for ray crystallographic analysis, and single crystal diffraction data are collected on Rigaku SCX diffractometer, by graphite monochromator monochromatization
Mok alpha ray (), 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 this fluorescent material is shown in Fig. 1 (using Diamond Software on Drawing).
Embodiment 2
By FDCA and the potassium nitrate of 0.202g, the europium nitrate mixing of 0.892g of 0.312g, it is subsequently adding
In 100ml acetonitrile solution, stirring 10 minutes, be then placed in the baking oven of 120 DEG C after static 48h, cooling obtains colourless block
Shape crystal, is red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n。
Red fluorescence material [the Eu that above-described embodiment is prepared3K2(FDA)4(NO3)3(MeCN)2]nCarry out fluorometric investigation,
It produces the red fluorescence of 70000a.u. intensity under the incident illumination of 395nm irradiates, and obtains fluorescent spectrum curve result such as Fig. 2
Shown in.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be as the criterion.
Claims (3)
1. a red fluorescence material, it is characterised in that this fluorescent material is entitled: [Eu3K2(FDA)4(NO3)3(MeCN)2]n,
The molecular formula of this material is: C28H14N5O29Eu3K2, molecular weight is 1418.55, and FDA is FDCA, crystal structure number
According to being shown in Table one, relevant bond distance's bond angle is shown in Table two；[Eu3K2(FDA)4(NO3)3(MeCN)2]nProduce under the incident illumination of 395nm irradiates
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. the preparation method of a red fluorescence material, it is characterised in that for preparing the red fluorescence material described in claim 1
Material [Eu3K2(FDA)4(NO3)3(MeCN)2]n, comprise the following steps:
FDCA, potassium nitrate and europium nitrate are mixed, is then added in acetonitrile solution, at 120 DEG C after stirring
Under the conditions of reaction obtain colourless bulk crystals, be red fluorescence material [Eu3K2(FDA)4(NO3)3(MeCN)2]n；This phosphor
Expect launch the red fluorescence of 70000a.u. intensity under the incident illumination of 395nm wavelength irradiates.
The preparation method of a kind of red fluorescence material the most according to claim 2, it is characterised in that the use of described each raw material
Amount is:
2,5-furandicarboxylic acid 0.156～0.312 weight portion, potassium nitrate 0.101～0.202 weight portion, europium nitrate 0.446～
0.892 weight portion, acetonitrile solution 40～80 weight portion；
Described mix after under conditions of 120 DEG C reaction obtain colourless bulk crystals and be: stir 10 minutes, be then placed on 120 DEG C
In baking oven after static 48h, cooling obtains colourless bulk crystals.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957328A (en) * | 2017-04-17 | 2017-07-18 | 北京石油化工学院 | A kind of fluorescent material glowed and preparation method thereof |
| CN106957649A (en) * | 2017-04-17 | 2017-07-18 | 北京石油化工学院 | A kind of fluorescent material of green light and preparation method thereof |
| CN108913125A (en) * | 2018-09-29 | 2018-11-30 | 北京石油化工学院 | A kind of red fluorescence material and preparation method thereof |
| CN109053776A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of green terbium base fluorescent material and preparation method thereof |
| CN109053775A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of red europium base fluorescent material and preparation method thereof |
| CN109053774A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of green fluorescence Inorganic-organic Hybrid Material and preparation method thereof |
| CN109111473A (en) * | 2018-10-18 | 2019-01-01 | 北京石油化工学院 | A kind of red fluorescence Inorganic-organic Hybrid Material and preparation method thereof |
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| FA-NIAN SHI ET AL.: "Synthesis and characterization of polymorphs of photoluminescent Eu(III)-(2,5-furandicarboxylic acid, oxalicacid)MOFs", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
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| 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 |
| CN106957649A (en) * | 2017-04-17 | 2017-07-18 | 北京石油化工学院 | A kind of fluorescent material of green light and preparation method thereof |
| CN106957328A (en) * | 2017-04-17 | 2017-07-18 | 北京石油化工学院 | A kind of fluorescent material glowed and preparation method thereof |
| CN108913125A (en) * | 2018-09-29 | 2018-11-30 | 北京石油化工学院 | A kind of red fluorescence material and preparation method thereof |
| CN108913125B (en) * | 2018-09-29 | 2021-04-06 | 北京石油化工学院 | Red fluorescent material and preparation method thereof |
| CN109053776A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of green terbium base fluorescent material and preparation method thereof |
| CN109111473A (en) * | 2018-10-18 | 2019-01-01 | 北京石油化工学院 | A kind of red fluorescence Inorganic-organic Hybrid Material and preparation method thereof |
| CN109053774A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of green fluorescence Inorganic-organic Hybrid 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 |
| CN109053775A (en) * | 2018-10-18 | 2018-12-21 | 北京石油化工学院 | A kind of red europium base 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 |
| 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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| CN105733560B (en) | 2018-02-23 |
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