CN109020998B - Green fluorescent material and preparation method thereof - Google Patents

Green fluorescent material and preparation method thereof Download PDF

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CN109020998B
CN109020998B CN201811145968.8A CN201811145968A CN109020998B CN 109020998 B CN109020998 B CN 109020998B CN 201811145968 A CN201811145968 A CN 201811145968A CN 109020998 B CN109020998 B CN 109020998B
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dmso
fluorescent material
fda
green fluorescent
ethanol
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CN109020998A (en
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王浩
王传奕
赵晨祺
郭文莉
李树新
伍一波
商育伟
杨丹
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Beijing Institute of Petrochemical Technology
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    • C07ORGANIC CHEMISTRY
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
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Abstract

The invention discloses green fluorescenceThe name of the fluorescent material is Eu3(FDA)4(DMSO)2(NO3)(H2O)2The molecular formula of the fluorescent material is as follows: c28H24NO27Eu3S2Molecular weight is 1326.48, FDA is 2, 5-furandicarboxylic acid, DMSO is dimethyl sulfoxide. The preparation method comprises the steps of mixing 2, 5-furandicarboxylic acid and europium nitrate, adding the mixture into a mixed solution of DMSO and ethanol, stirring, and reacting at 120 ℃ to obtain colorless blocky crystals. The fluorescent material can emit green fluorescence with the intensity of 6000000a.u. under the irradiation of incident light with the wavelength of 380 nm. The invention can synthesize functional materials with excellent green fluorescence performance, has longer service life and higher color purity, and has simple preparation method, easy control of chemical components, good repeatability and high yield.

Description

Green fluorescent material and preparation method thereof
Technical Field
The invention relates to the field of fluorescent materials, in particular to a green fluorescent material and a preparation method thereof.
Background
Modern fluorescent materials have become support materials in the fields of information display, lighting sources, photoelectric devices and the like, and can be widely applied in the fields of luminous ink, luminous paint, luminous plastics, luminous printing paste, organic pigment, optical brightening agent, photo-oxidant, paint, chemical and biochemical analysis, solar collectors, anti-counterfeiting marks, medicine tracing, laser and the like. However, the existing fluorescent materials, especially green fluorescent materials, have short service life and low color purity, and the existing green luminescent materials have complex preparation methods and high cost.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a green fluorescent material and a preparation method thereof, which can synthesize a functional material with excellent green fluorescence performance, and have the advantages of longer service life, higher color purity, simple preparation method, easy control of chemical components, good repeatability, high yield and low cost.
The purpose of the invention is realized by the following technical scheme:
a green fluorescent material, the name of the fluorescent material is: tb3(FDA)4(DMSO)2(NO3)(H2O)2The molecular formula of the material is as follows: c28H24NO27Tb3S2The molecular weight is 1347.36, FDA is 2, 5-furandicarboxylic acid, DMSO is dimethyl sulfoxide, the crystal structure data is shown in a table I, and the bond angle of the relevant bond length is shown in a table II; tb3(FDA)4(DMSO)2(NO3)(H2O)2Green fluorescence with an intensity of 6000000a.u. under irradiation of incident light at 380 nm;
the first table is as follows: tb3(FDA)4(DMSO)2(NO3)(H2O)2Crystallographic parameters of
Figure BDA0001816814000000011
Figure BDA0001816814000000021
The second table is: tb3(FDA)4(DMSO)2(NO3)(H2O)2Length of the bond
Figure BDA0001816814000000022
Angle of harmony key (°)
Figure BDA0001816814000000023
Figure BDA0001816814000000031
Symmetric code: (i) x, -y +1, z + 1/2; (ii) -x +1/2, y +1/2, -z + 1/2; (iii) x, -y, z + 1/2; (iv) -x +1, -y, -z + 1; (v) x, -y, z-1/2; (vi) x, -y +1, z-1/2; (vii) -x +1/2, y-1/2, -z + 1/2; (viii) -x +1, y, -z + 1/2.
The invention also provides a preparation method of the green fluorescent material, which is used for preparing the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2The method specifically comprises the following steps:
mixing 2, 5-furandicarboxylic acid and terbium nitrate, adding the mixture into a mixed solution of DMSO and ethanol (the volume ratio of the DMSO to the ethanol is 1:1), stirring, and reacting at 120 ℃ to obtain a colorless blocky crystal which is the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2(ii) a The fluorescent material can emit green fluorescence with the intensity of 6000000a.u. under the irradiation of incident light with the wavelength of 380 nm.
In the preparation method, the dosage ratio of the raw materials is as follows: 0.156-0.312 part of 2, 5-furandicarboxylic acid, 0.453-0.906 part of terbium nitrate and 40-80 parts of mixed solution of DMSO and ethanol.
Preferably, the reaction carried out at 120 ℃ after stirring to obtain colorless bulk crystals may be: stirred for 10 minutes, then placed in an oven at 120 ℃ for standing for 48 hours, and then cooled, thereby obtaining colorless massive crystals.
The invention has at least the following beneficial effects: the embodiment of the invention adopts a solvent thermal synthesis mode to prepare the functional material with excellent green fluorescence performance, the preparation process is simple, the chemical components are easy to control, the repeatability is good, the yield is high, the raw materials are easy to obtain, the cost is low, and the prepared green fluorescence material has longer service life, higher color purity and better fluorescence performance compared with the existing green fluorescence material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a crystal structure diagram of a green fluorescent material according to an embodiment of the present invention.
Fig. 2 is a fluorescence spectrum of the green fluorescent material according to the embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The green fluorescent material and the preparation method thereof provided by the present invention are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
Example 1
A green light-emitting fluorescent material is prepared by the following method: mixing 0.156g of 2, 5-furandicarboxylic acid and 0.453g of terbium nitrate, then adding the mixture into 40g of mixed solution of DMSO and ethanol (the volume ratio of the DMSO to the ethanol is 1:1), stirring the mixture for 10 minutes, placing the mixture in an oven at 120 ℃ for standing for 48 hours, and then cooling the mixture to obtain colorless blocky crystals, namely the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2
Specifically, the dimensions are selected to be 0.26 × 0.25 × 0.23mm3The fluorescent material is subjected to single crystal structure analysis, single crystal diffraction data are collected by a Bruker-AXS SMART APEX2CCD diffractometer, and Mok alpha rays are monochromatized by a graphite monochromator
Figure BDA0001816814000000042
Theta is 1.7 DEG-25.2 DEG, so that the following results are obtained: the fluorescent material belongs to a monoclinic system, the space group is C2/C, and the unit cell parameter is about
Figure BDA0001816814000000041
α is 90 °, β is 113.484 °, and γ is 90 °. The crystal structure of the fluorescent material was plotted using Diamond software, resulting in a schematic crystal structure as shown in fig. 1.
Example 2
A green light-emitting fluorescent material is prepared by the following method: mixing 0.312g of 2, 5-furandicarboxylic acid and 0.906g of terbium nitrate, then adding the mixture into 80g of mixed solution of DMSO and ethanol (the volume ratio of the DMSO to the ethanol is 1:1), stirring the mixture for 10 minutes, placing the mixture in an oven at 120 ℃ for standing for 48 hours, and then cooling the mixture to obtain colorless blocky crystals, namely the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2
Specifically, a single crystal diffractometer is adopted to perform fluorescence test on the fluorescent material emitting green light, and the wavelength of incident light is 380nm, so that a fluorescence spectrum curve shown in fig. 2 can be obtained; in FIG. 2, the abscissa is wavenumber (i.e., wavelength in nm) and the ordinate is intensity (i.e., intensity). As can be seen from fig. 2: the fluorescent material in embodiment 2 of the present invention can emit green fluorescence with an intensity of 6000000a.
In conclusion, the invention can synthesize the functional material with excellent green fluorescence performance, has longer service life, higher color purity, simple preparation method, easy control of chemical components, good repeatability, high yield and low cost.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (4)

1. A green fluorescent material characterized by the name: tb3(FDA)4(DMSO)2(NO3)(H2O)2The molecular formula of the material is as follows: c28H24NO27Tb3S2Molecular weight is 1347.36, FDA is 2, 5-furandicarboxylic acid, DMSO is dimethyl sulfoxide; the crystal structure data is shown in the following table I, and the relevant bond length and bond angle is shown in the following table II; the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2Green fluorescence with an intensity of 6000000a.u. under irradiation of incident light at 380 nm;
the first table is as follows: tb3(FDA)4(DMSO)2(NO3)(H2O)2Crystallographic parameters of
Figure FDA0001816813990000011
The second table is: tb3(FDA)4(DMSO)2(NO3)(H2O)2Length of the bond
Figure FDA0001816813990000013
Angle of harmony key (°)
Figure FDA0001816813990000012
Figure FDA0001816813990000021
Figure FDA0001816813990000031
Symmetric code: (i) x, -y +1, z + 1/2; (ii) -x +1/2, y +1/2, -z + 1/2; (iii) x, -y, z + 1/2; (iv) -x +1, -y, -z + 1; (v) x, -y, z-1/2; (vi) x, -y +1, z-1/2; (vii) -x +1/2, y-1/2, -z + 1/2; (viii) -x +1, y, -z + 1/2.
2. A method for preparing a green fluorescent material, characterized by preparing the green fluorescent material Tb described in claim 13(FDA)4(DMSO)2(NO3)(H2O)2The method comprises the following steps:
mixing 2, 5-furandicarboxylic acid and terbium nitrate, adding the mixture into a mixed solution of DMSO and ethanol, stirring the mixture, and reacting the mixture at 120 ℃ to obtain a colorless blocky crystal which is the green fluorescent material Tb3(FDA)4(DMSO)2(NO3)(H2O)2(ii) a The fluorescent material can emit green fluorescence with the intensity of 6000000a.u. under the irradiation of incident light with the wavelength of 380 nm;
the mixed solution of DMSO and ethanol is formed by mixing DMSO and ethanol according to the volume ratio of 1: 1.
3. The method for preparing a green fluorescent material according to claim 2, wherein the ratio of the amounts of the raw materials is: 0.156-0.312 part of 2, 5-furandicarboxylic acid, 0.453-0.906 part of terbium nitrate and 40-80 parts of mixed solution of DMSO and ethanol.
4. The method of claim 2 or 3, wherein the reacting at 120 ℃ after stirring to obtain the colorless bulk crystal comprises: stirred for 10 minutes, then placed in an oven at 120 ℃ for standing for 48 hours, and then cooled, thereby obtaining colorless massive crystals.
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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
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
CN107603600A (en) * 2017-10-01 2018-01-19 桂林理工大学 A kind of terbium coordination compound green luminescent material and synthetic method
CN108558917A (en) * 2018-05-29 2018-09-21 江西省科学院应用化学研究所 A kind of zinc-furandicarboxylic acid organic framework materials and preparation method

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US8269029B2 (en) * 2008-04-08 2012-09-18 The Board Of Trustees Of The University Of Illinois Water repellent metal-organic frameworks, process for making and uses regarding same

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
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
CN107603600A (en) * 2017-10-01 2018-01-19 桂林理工大学 A kind of terbium coordination compound green luminescent material and synthetic method
CN108558917A (en) * 2018-05-29 2018-09-21 江西省科学院应用化学研究所 A kind of zinc-furandicarboxylic acid organic framework materials and preparation method

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