CN102617616A - Microwave radiation method for preparing cerium metal organic light-emitting material - Google Patents
Microwave radiation method for preparing cerium metal organic light-emitting material Download PDFInfo
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- CN102617616A CN102617616A CN2012100419622A CN201210041962A CN102617616A CN 102617616 A CN102617616 A CN 102617616A CN 2012100419622 A CN2012100419622 A CN 2012100419622A CN 201210041962 A CN201210041962 A CN 201210041962A CN 102617616 A CN102617616 A CN 102617616A
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- microwave
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- phenanthroline
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- pyrazine
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Abstract
A microwave radiation method for preparing a cerium metal organic light-emitting material relates to preparation of organic light-emitting materials. The microwave radiation method is characterized in that 2,3-dicarboxylic acid-pyrazine [4,5-f]1,10-phenanthroline cerium metal organic light-emitting material complex is produced by the microwave radiation method, and the material has a general formula shown in an instruction book, R1 refers to H, C6H5, C6H60, C6H7O2 and CHO2, R2 refers to H, C6H5, C6H6O, C6H7O2 and CHO2, and n=1-4. Both Ce (NO3) 3.6 H2O and 2,3-dicarboxylic acid-pyrazine [4,5-f]1,10-phenanthroline are solids and are proportionally mixed, and then the cerium metal organic light-emitting material complex is prepared by means of microwave heating reaction. The microwave radiation method has the advantages of high efficiency and less pollution, and the complex is a worthy potential light-emitting material.
Description
Technical field
The present invention relates to prepare a kind of luminous organic material, particularly relate to the microwave solid phase method and prepare a kind of metallic cerium luminous organic material.
Background technology
Because rare earth has the 4f electronic structure of underfilling; Make it because it has good physical propertys such as photo-electro-magnetic; Type material that can be different, various in style with the other materials component property, its most significant function is exactly quality and the performance that increases substantially other products.Such as the performance that increases substantially steel, duraluminum, magnesiumalloy, titanium alloy.And rare earth is many high-tech promotor such as electronics, laser, superconduction equally, and is especially outstanding with rare earth luminescent material.Cerium is applied to every field widely as the rare earth that practical use is arranged the earliest, and luminescent material is the importance that cerium is used, but how to participate with oxide form.Therefore, carry out and utilize organic ligand that the study on the modification of cerium ion is had great importance.
Microwave is the hertzian wave that comprises electric field and magnetic field; Its electric field produces reactive force to charged particle and makes it migration or rotation; Its heating has pyrogenicity and two kinds of effects of non-pyrogenicity; The former makes reactant molecule motion aggravation and the temperature rising, and the latter is then from the Lorentz force action of microwave field to ion and polar molecule.Microwave heating has 3 characteristics: ability rapid heating when (1) a large amount of ions exist; (2) arrive temperature of reaction fast; (3) stirring under the molecular level meaning.Because microwave is on molecular level, to heat, thereby has accelerated speed of response.Many speed of response tens of times of popular response often under microwave catalysis, even thousands of times.Because it is fast that microwave chemical reaction exists speed, yield is high, and the product separate easily is polluted advantages such as little or pollution-free, more and more receives people's attention, uses extensive just day by day.Microwave is in the application in rare earth chemistry field, for making the brand-new platform that advanced luminescent material provides.
Summary of the invention
The object of the present invention is to provide the microwave solid phase method to prepare a kind of metallic cerium luminous organic material, through changing the mol ratio of material, with solid phase synthesis technique; Preparation imidazoles 2,3-dicarboxylicacid-pyrazine [4,5-f] 1; The method of 10-phenanthroline cerium complexes makes a kind of rare earth compounding of novelty.This title complex is a kind of valuable potential luminescent material.
The present invention realizes through following technical scheme:
The microwave solid phase method prepares a kind of metallic cerium luminous organic material, and its said material adopts the microwave solid phase method to produce 2,3-dicarboxylicacid-pyrazine [4,5-f] 1, and 10-phenanthroline cerium metal luminous organic material title complex has following general formula:
Wherein: R
1Be H, C
6H
5, C
6H
6O, C
6H
7O
2, CHO
2; R
2Be H, C
6H
5, C
6H
6O, C
6H
7O
2, CHO
2; N=1-4.
Described microwave solid phase method prepares a kind of metallic cerium luminous organic material, its described Ce (NO
3)
3.6H
2O and 2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the 10-phenanthroline is solid, behind the proportional mixing, through the microwave heating reaction, makes cerium metal luminous organic material title complex.
Described microwave solid phase method prepares a kind of metallic cerium luminous organic material, and the purposes of its described cerium metal luminous organic material title complex is for being used to make the fluorescence luminescent material aspect; Or be used to prepare the rare earth metal luminous organic material.
A kind of 2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the preparation method of 10-phenanthroline cerium complexes is:
Take by weighing 2,3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline and Pottasium Hydroxide (KOH) mol ratio is 1:2; Add the beaker that water is housed, stirring lets it fully react, and is heated to then about 70 ℃, with the water evaporate to dryness; Obtain 2,3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline sylvite.
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:1) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven, microwave power 200-800W after 5 minutes, closes microwave oven; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.The fluorescence intensity of this product reaches 583, and the maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Description of drawings
Fig. 1 is an imidazoles [4,5-f] 1,10-phenanthroline cerium complexes excite collection of illustrative plates;
Fig. 2 is an imidazoles [4,5-f] 1, the emission collection of illustrative plates of 10-phenanthroline cerium complexes.
Annotate: Fig. 1-Fig. 2 of the present invention is the analysis synoptic diagram of product state, the unintelligible understanding that does not influence technical scheme of the present invention of figure Chinese words.
Embodiment
Below in conjunction with embodiment the present invention is elaborated.
Embodiment 1:
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:1) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven,, after 10 minutes, close microwave oven at microwave power 200-800W; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.This product maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Embodiment 2:
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:1) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven,, after 20 minutes, close microwave oven at microwave power 200-800W; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.This product maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Embodiment 3:
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:1) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven,, after 30 minutes, close microwave oven at microwave power 200-800W; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.This product maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Embodiment 4:
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:2) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven,, after 5 minutes, close microwave oven at microwave power 200-800W; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.This product maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Embodiment 5:
With rare earth nitrate (Ce (NO
3)
3.6H
2O) utilize mechanical stirring mixing (rare earth nitrate and part mol ratio are 1:3) with part (2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the sylvite of 10-phenanthroline); Then mixture is put into microwave oven,, after 5 minutes, close microwave oven at microwave power 200-800W; Be cooled to room temperature, products therefrom is used water washing, and oven dry obtains 2; 3-dicarboxylicacid-pyrazine [4,5-f] 1,10-phenanthroline cerium complexes.This product maximum excitation wavelength is 625nm, and maximum emission wavelength is 487nm.
Claims (3)
1. the microwave solid phase method prepares a kind of metallic cerium luminous organic material, it is characterized in that, said material adopts the microwave solid phase method to produce 2,3-dicarboxylicacid-pyrazine [4,5-f] 1, and 10-phenanthroline cerium metal luminous organic material title complex has following general formula:
Wherein: R
1Be H, C
6H
5, C
6H
6O, C
6H
7O
2, CHO
2; R
2Be H, C
6H
5, C
6H
6O, C
6H
7O
2, CHO
2; N=1-4.
2. microwave solid phase method according to claim 1 prepares a kind of metallic cerium luminous organic material, it is characterized in that, described Ce (NO
3)
3.6H
2O and 2,3-dicarboxylicacid-pyrazine [4,5-f] 1, the 10-phenanthroline is solid, behind the proportional mixing, through the microwave heating reaction, makes cerium metal luminous organic material title complex.
3. microwave solid phase method according to claim 1 prepares a kind of metallic cerium luminous organic material, it is characterized in that, the purposes of described cerium metal luminous organic material title complex is for being used to make the fluorescence luminescent material aspect; Or be used to prepare the rare earth metal luminous organic material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617617A (en) * | 2012-02-23 | 2012-08-01 | 沈阳化工大学 | Imidazo[4,5-f]1,10-phenanthroline cerium complex and preparation method thereof |
| CN106832326A (en) * | 2017-03-28 | 2017-06-13 | 河北医科大学 | A kind of high-thermal-stability cerium coordination polymer and its preparation method and application |
| CN109370410A (en) * | 2018-09-28 | 2019-02-22 | 合众（佛山）化工有限公司 | A kind of high performance nanometer energy storage aqueous luminous paint |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617617A (en) * | 2012-02-23 | 2012-08-01 | 沈阳化工大学 | Imidazo[4,5-f]1,10-phenanthroline cerium complex and preparation method thereof |
-
2012
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617617A (en) * | 2012-02-23 | 2012-08-01 | 沈阳化工大学 | Imidazo[4,5-f]1,10-phenanthroline cerium complex and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| XIAO-NING ZHANG ET AL.: ""Synthesis, Structures, and Properties of Two Novel Supramolecular Architectures Constructed from [2,3f]Pyrazino[1,10]phenanthroline-2,3-dicarboxylic Acid"", 《Z. ANORG. ALLG. CHEM》 * |
| XIAO-NING ZHANG ET AL.: ""Synthesis, Structures, and Properties of Two Novel Supramolecular Architectures Constructed from [2,3f]Pyrazino[1,10]phenanthroline-2,3-dicarboxylic Acid"", 《Z. ANORG. ALLG. CHEM》, vol. 635, 31 December 2009 (2009-12-31), pages 2622 - 2626 * |
| ZHEHUI WENG ET AL.: ""Two Types of Lanthanide Coordination Polymers of (2,3-f)-Pyrazino(1,10)phenanthroline-2,3-dicarboxylic Acid: Syntheses，Structures, and Properties"", 《CRYSTAL GROWTH AND DESIGN》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617617A (en) * | 2012-02-23 | 2012-08-01 | 沈阳化工大学 | Imidazo[4,5-f]1,10-phenanthroline cerium complex and preparation method thereof |
| CN106832326A (en) * | 2017-03-28 | 2017-06-13 | 河北医科大学 | A kind of high-thermal-stability cerium coordination polymer and its preparation method and application |
| CN106832326B (en) * | 2017-03-28 | 2019-11-05 | 河北医科大学 | A kind of high-thermal-stability cerium coordination polymer and its preparation method and application |
| CN109370410A (en) * | 2018-09-28 | 2019-02-22 | 合众（佛山）化工有限公司 | A kind of high performance nanometer energy storage aqueous luminous paint |
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Application publication date: 20120801 |