CN109053776A - A kind of green terbium base fluorescent material and preparation method thereof - Google Patents

A kind of green terbium base fluorescent material and preparation method thereof Download PDF

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Publication number
CN109053776A
CN109053776A CN201811217034.0A CN201811217034A CN109053776A CN 109053776 A CN109053776 A CN 109053776A CN 201811217034 A CN201811217034 A CN 201811217034A CN 109053776 A CN109053776 A CN 109053776A
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China
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dmac
fluorescent material
green
fda
base fluorescent
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CN109053776B (en
Inventor
王浩
王传奕
全葳
吴浩东
郭文莉
李树新
伍波
伍一波
商育伟
杨丹
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Beijing Institute of Petrochemical Technology
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Beijing Institute of Petrochemical Technology
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00Compounds containing elements of Groups 3 or 13 of the Periodic System
    • C07F5/003Compounds containing elements of Groups 3 or 13 of the Periodic System without C-Metal linkages
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2211/00Chemical nature of organic luminescent or tenebrescent compounds
    • C09K2211/18Metal complexes
    • C09K2211/182Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide

Abstract

The invention discloses a kind of green terbium base fluorescent materials and preparation method thereof, which is Tb2(FDA)3(DMAC)2·(H2O), FDA is 2,5-furandicarboxylic acid, and DMAC is dimethyl acetamide.Preparation method is to mix 2,5-furandicarboxylic acid with terbium nitrate, is then added in the mixed solution of DMAC, second alcohol and water, and reacted after agitation with 100 DEG C, so that colourless bulk crystals be made.The fluorescent material generates the green fluorescence of 9000000a.u. intensity under the incident light irradiation of 365nm.The present invention can synthesize the functional material that fluoresced green is had excellent performance, and there are longer life expectancy, excitation purity are higher, and preparation method is simple, chemical constituent is easily controllable, reproducible, yield is high.

Description

A kind of green terbium base fluorescent material and preparation method thereof
Technical field
The present invention relates to fluorescent material technical fields more particularly to a kind of green terbium base fluorescent material and preparation method thereof.
Background technique
Modern fluorescence material have become information show, the backing material in the fields such as lighting source, photoelectric device, can make Luminous printing ink, luminous paint, luminescent plastic, shine printing paste, organic pigment, Optical Bleaching Agent, photooxidant, coating, chemistry And the fields such as biochemical analysis, solar energy trap, anti-fake mark, pharmaceutical indications and laser have obtained wider application.But it is existing Some fluorescent materials, especially green fluorescent material are short there are the service life, excitation purity is not high, and existing green luminescent material Preparation method is complicated, at high cost.
Summary of the invention
For above-mentioned shortcoming in the prior art, the present invention provides a kind of green terbium base fluorescent material and its preparations Method can synthesize the functional material that fluoresced green is had excellent performance, there are longer life expectancy, excitation purity are higher, and preparation side Method is simple, chemical constituent is easily controllable, reproducible, yield is high, low in cost.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of green terbium base fluorescent material, the title material are as follows: Tb2(FDA)3(DMAC)2·(H2O), the material molecule formula Are as follows: C26H26N2O18Tb2, molecular weight 972.31, FDA is 2,5-furandicarboxylic acid, and DMAC is dimethyl acetamide, crystal structure Data are shown in Table one, and related bond distance's bond angle is shown in Table two;Tb2(FDA)3(DMAC)2·(H2O it) is generated under the incident light irradiation of 365nm 9000000a.u. the green fluorescence of intensity;
Table one are as follows: Tb2(FDA)3(DMAC)2·(H2O crystallographic parameter)
Table two are as follows: Tb2(FDA)3(DMAC)2·(H2O bond distance)With bond angle (°)
Symmetrical code: (i)-x ,-y+1 ,-z+1;(ii)-x-1,-y+1,-z+1;(iii)x+1,y,z-1;(iv)-x+1,- y,-z+1;(v)-x+1,-y,-z;(vi)x+1,y-1,z;(vii)-x,-y+1,-z;(viii)x-1,y+1,z;(ix)x-1,y, z+1.
The present invention also provides a kind of preparation methods of green terbium base fluorescent material, are used to prepare green terbium of the present invention Base fluorescent material Tb2(FDA)3(DMAC)2·(H2O), it can specifically include following steps:
2,5-furandicarboxylic acid and terbium nitrate are mixed, be then added to DMAC, second alcohol and water mixed solution (DMAC, Ethyl alcohol, water volume ratio be 1:1:1) in, and carry out reaction so that colourless bulk crystals be made, as with 100 DEG C after agitation Green terbium base fluorescent material Tb2(FDA)3(DMAC)2·(H2O);Fluorescent material energy under the incident light irradiation of 365nm wavelength Launch the green fluorescence of 9000000a.u. intensity.
In above-mentioned preparation method, the ratio between the dosage of each raw material are as follows: 0.156~0.312 parts by weight of 2,5-furandicarboxylic acid, nitre Sour 0.453~0.906 parts by weight of terbium, 40~80 parts by weight of mixed solution of DMAC, second alcohol and water.
Preferably, it is described carry out reaction after agitation with 100 DEG C can be with to which colourless bulk crystals be made are as follows: 10 points of stirring Then clock is placed on static 48h in 100 DEG C of baking oven, then is cooled down, so that colourless bulk crystals be made.
The present invention at least has following beneficial effect: the embodiment of the present invention can prepare greening using solvent-thermal process mode The excellent functional material of color fluorescence property, preparation process is simple, chemical constituent is easily controllable, reproducible, yield is high, raw material is easy It obtains, is low in cost, and there are longer life expectancy, colour purity than existing green fluorescent material for green fluorescent material obtained by the present invention Du Genggao, fluorescence property are more preferable.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other Attached drawing.
Fig. 1 is the crystal structure figure of green terbium base fluorescent material provided in an embodiment of the present invention.
Fig. 2 is fluorescence spectra provided in an embodiment of the present invention.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts Example, belongs to protection scope of the present invention.
Green terbium base fluorescent material provided by the present invention and preparation method thereof is described in detail below.The present invention is real It applies the content being not described in detail in example and belongs to the prior art well known to professional and technical personnel in the field.
Embodiment 1
A kind of green terbium base fluorescent material, is made of following methods: by the 2,5-furandicarboxylic acid of 0.156g and The terbium nitrate of 0.453g mixes, and is then added to the DMAC of 40g, the mixed solution (volume of DMAC, ethyl alcohol, water of second alcohol and water Than in 1:1:1), and it is placed on static 48h in 100 DEG C of baking oven after ten minutes in stirring, then cooled down, to be made colourless Bulk crystals, as green terbium base fluorescent material Tb2(FDA)3(DMAC)2·(H2O)。
Specifically, selection is having a size of 0.25 × 0.24 × 0.23mm3The green terbium base fluorescent material carry out monocrystalline knot Structure analysis, single crystal diffraction data are collected using Bruker-AXS SMART APEX2CCD diffractometer, with graphite monochromator list The Mok alpha ray of color, 2.7 °≤θ≤25.1 °, to obtain following result: the fluorescent material category In anorthic system, space group is all P-1, and cell parameter is about α=80.25 °, β=73.93 °, γ=74.40 °.Use the crystal knot of the Diamond Software on Drawing fluorescent material Structure obtains crystal structure schematic diagram as shown in Figure 1.
Embodiment 2
A kind of green terbium base fluorescent material, is made of following methods: by the 2,5-furandicarboxylic acid of 0.312g and The terbium nitrate of 0.906g mixes, and is then added to the DMAC of 80g, the mixed solution (volume of DMAC, ethyl alcohol, water of second alcohol and water Than in 1:1:1), and it is placed on static 48h in 100 DEG C of baking oven after ten minutes in stirring, then cooled down, to be made colourless Bulk crystals, as green terbium base fluorescent material Tb2(FDA)3(DMAC)2·(H2O)。
Specifically, fluorometric investigation is carried out to the fluorescent material to glow using single crystal diffractometer, incident light wave is a length of 365nm, so as to obtain fluorescent spectrum curve as shown in Figure 2;In Fig. 2, abscissa is wavenumber (as wave It is long, unit nm), ordinate is intensity (as intensity).As seen from Figure 2: glimmering in the embodiment of the present invention 2 Luminescent material can launch the green fluorescence of 9000000a.u. intensity under the incident light irradiation of 365nm wavelength.
To sum up, the present invention can synthesize the functional material that fluoresced green is had excellent performance, and there are longer life expectancy, colour purity Du Genggao, and preparation method is simple, chemical constituent is easily controllable, reproducible, yield is high, low in cost.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Subject to enclosing.

Claims (4)

1. a kind of green terbium base fluorescent material, which is characterized in that Tb2(FDA)3(DMAC)2·(H2O), the material molecule formula are as follows: C26H26N2O18Tb2, FDA is 2,5-furandicarboxylic acid, and DMAC is dimethyl acetamide;Its crystal structural data see the table below one, Related bond distance's bond angle see the table below two;Green terbium base fluorescent material Tb2(FDA)3(DMAC)2·(H2O) in the incident light of 365nm The lower green fluorescence for generating 9000000a.u. intensity of irradiation;
Table one are as follows: Tb2(FDA)3(DMAC)2·(H2O crystallographic parameter)
Table two are as follows: Tb2(FDA)3(DMAC)2·(H2O bond distance)With bond angle (°)
Symmetrical code: (i)-x ,-y+1 ,-z+1;(ii)-x-1,-y+1,-z+1;(iii)x+1,y,z-1;(iv)-x+1,-y,-z +1;(v)-x+1,-y,-z;(vi)x+1,y-1,z;(vii)-x,-y+1,-z;(viii)x-1,y+1,z;(ix)x-1,y,z+1.
2. a kind of preparation method of green terbium base fluorescent material, which is characterized in that be used to prepare described in the claims 1 Green terbium base fluorescent material Tb2(FDA)3(DMAC)2·(H2O), comprising the following steps:
2,5-furandicarboxylic acid is mixed with terbium nitrate, is then added in the mixed solution of DMAC, second alcohol and water, and stirring It is reacted afterwards with 100 DEG C, so that colourless bulk crystals are made, as green terbium base fluorescent material Tb2(FDA)3(DMAC)2· (H2O);The fluorescent material can launch the green fluorescence of 9000000a.u. intensity under the incident light irradiation of 365nm wavelength;
Wherein, the DMAC, second alcohol and water mixed solution be by DMAC, second alcohol and water alcohol according to 1:1:1 volume ratio mix Made of.
3. the preparation method of green terbium base fluorescent material according to claim 2, which is characterized in that the use of each raw material The ratio between amount are as follows: 0.156~0.312 parts by weight of 2,5-furandicarboxylic acid, 0.453~0.906 parts by weight of terbium nitrate, DMAC, ethyl alcohol With 40~80 parts by weight of mixed solution of water.
4. the preparation method of green terbium base fluorescent material according to claim 2 or 3, which is characterized in that described to stir Carrying out reaction with 100 DEG C afterwards to which colourless bulk crystals be made includes: stirring 10 minutes, is then placed on quiet in 100 DEG C of baking oven Only 48h, then cooled down, so that colourless bulk crystals be made.
CN201811217034.0A 2018-10-18 2018-10-18 Green terbium-based fluorescent material and preparation method thereof Active CN109053776B (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
CN105694858A (en) * 2016-03-18 2016-06-22 北京石油化工学院 Green fluorescent material and preparation method of green fluorescent material
CN105733560A (en) * 2016-03-18 2016-07-06 北京石油化工学院 Red fluorescent material and method for preparing same
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105694858A (en) * 2016-03-18 2016-06-22 北京石油化工学院 Green fluorescent material and preparation method of green fluorescent material
CN105733560A (en) * 2016-03-18 2016-07-06 北京石油化工学院 Red fluorescent material and method for preparing same
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PENG CHENG ET AL.: "Highly Selective Sorption and Luminescent Sensing of Small Molecules Demonstrated in a Multifunctional Lanthanide Microporous Metal–Organic Framework Containing 1D Honeycomb-Type Channels", 《CHEM. EUR. J.》 *

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