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Organic rare earth europium light-emitting dacron and preparation method thereof

A rare earth and organic technology, applied in the direction of luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problem of poor energy level matching, low luminous intensity of complexes, oxidation resistance, color purity, luminous efficiency and Problems such as poor luminous intensity, to achieve the effect of preventing fluorescence quenching, good luminous intensity, and improving spinnability

Active Publication Date: 2015-05-13
湖州信倍连网络科技有限公司
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Problems solved by technology

Eu(BA) 3 (TPPO) 2 Doped in PVP (Poly Vinyl Pyrrolidone, polyvinylpyrrolidone) for composite spinning, prepared composite nanofibers with strong anti-bleaching ability and stable luminescence; because the energy level matching between the ligand and Eu(Ⅲ) ions is not very good , the luminescence intensity of the resulting complex is not very high
Chinese patent CN101381901A, application number: 200810042269.0, prepared a series of organic small molecule fluorescent compounds doped into polypropylene for melt spinning, and prepared polypropylene light emitting fibers with good luminous performance and different luminous colors; Molecularly prepared fibers have poor oxidation resistance, color purity, luminous efficiency and luminous intensity

Method used

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  • Organic rare earth europium light-emitting dacron and preparation method thereof
  • Organic rare earth europium light-emitting dacron and preparation method thereof
  • Organic rare earth europium light-emitting dacron and preparation method thereof

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preparation example Construction

[0044] The present invention also provides a preparation method of an organic rare earth europium complex luminescent material, comprising the following steps:

[0045] (1) Preparation of ligand 2,3-dimethylpyrazino[1,10]phenanthroline:

[0046] a. Put 1,10-phenanthroline and potassium bromide into a flask, add dropwise a mixed acid solution of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1-2 at -8°C to -12°C, React at 8°C to -12°C for 0.5-1.5h, heat to 75-95°C for 130-150min; drop the reaction solution into ice cubes, stir rapidly, adjust the pH to 6-7 with NaOH to obtain a neutralized solution, and use solvent extraction of the neutralized solution, and distillation under reduced pressure to obtain the yellow product 5,6-diketone-1,10-phenanthroline;

[0047] Add 0.4-1g potassium bromide for every 1g of 1,10-phenanthroline;

[0048] For every 1g of 1,10-phenanthroline, the corresponding mixed acid solution is 20-30ml;

[0049] The solve...

Embodiment 1

[0079] Rare earth europium complex Eu(TTA) 3 The preparation process of DMPaPhen is as follows:

[0080] Synthesis of 1,10-phenanthroline-5,6-dione (compound 1): Weigh 1g of 1,10-phenanthroline and 0.6g of potassium bromide into a 100mL two-necked flask, place the flask Cool to -10°C in an ice-salt bath. Measure 16mL of concentrated sulfuric acid and pour it into a 200mL beaker, then measure 8ml of concentrated nitric acid with a graduated cylinder. Slowly add concentrated nitric acid to the beaker with a dropper under the condition of an ice-salt bath, and stir with a glass rod while adding. The addition takes about 30 minutes. If the addition is too fast, it will smoke. After the acid solution is prepared, it is slowly added dropwise to the flask, and the dropwise addition process is kept at -10°C in an ice bath for about 0.5 hours. Then react in an ice bath for 1 hour, then program the temperature to 85° C., keep the reaction for 130 minutes, and cool to room temperature...

Embodiment 2

[0097] This example only illustrates the preparation of luminescent fibers with different contents of luminescent materials and different spinning process conditions. The preparation method of the luminescent materials is the same as in Example 1, and the preparation process of the luminescent fibers is as follows:

[0098] Fully mix the nano-scale luminescent material prepared above with the PET masterbatch, prepare a color masterbatch containing 5% of the organic rare earth complex with a twin-screw extruder, and dry it at 120°C for 12 hours in a vacuum (vacuum degree is 0.09MPa). Make its moisture content less than 20ppm.

[0099] The PET polyester chips are transported to the pre-crystallizer, the pre-crystallization temperature is set at 170-175°C, preferably 175°C, and the residence time of the pre-crystallization is 17-23min, preferably 23min. The material passed through the pre-crystallizer is continuously transported to the main drying tower, and the drying temperatur...

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Abstract

The invention discloses an organic rare earth europium light-emitting dacron and a preparation method thereof. The preparation method comprises the following steps: firstly preparing an o-phenanthroline neutral ligand which is combined with alpha-thenoyltrifluoroacetone and rare earth Eu (III) for coordination and preparing a rare earth europium coordination compound Eu(TTA)3DMPaPhen light-emitting material having a close nanoscale by virtue of an atmospheric titration and high-pressure reaction method. The material emits very strong pure red light in a 10<-5>mol / L CH2Cl2 solution at 615nm. A light-emitting fiber is prepared from the coordination compound as a light-emitting material and polyethylene terephthalate (PET) through composite melt spinning. When the content of the rare earth light-emitting material in the fiber is 0.05%, the rare earth light-emitting material emits very strong pure red light in a 10<-5>mol / L CH2Cl2 solution at a light-emitting position of 615nm. The light-emitting fiber has the advantages of high color purity and good spinnability.

Description

technical field [0001] The invention belongs to the fields of luminescent materials and textile science, and in particular relates to an organic rare earth europium luminescent polyester and a preparation method thereof. Background technique [0002] Rare earth elements are located in the lanthanide series of the periodic table of elements. Because of the same outer electron structure and similar inner 4f energy levels, rare earth elements exhibit many unique physical and chemical properties, so they are widely used in the fields of optics, electricity, and magnetism. application. In general, the fluorescence emission of rare earth ions mainly comes from the f-f electronic transition of the 4f electron shell, and the 5S 2 and 5P 6 The electrons generally shield the 4f electrons, so the matrix has little influence on the photoradiative transition of the 4f electron layer. This shielding effect can just make rare earth ions produce sharp band emission and long fluorescence ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C07F5/00D01F6/92D01F1/10
Inventor 顾玲袁欢欢提云崇徐国华顾昕
Owner 湖州信倍连网络科技有限公司
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