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Organic rare earth europium luminescent nylon and preparation method thereof

A rare earth and organic technology, applied in luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problems of oxidation resistance, color purity, luminous efficiency, poor luminous intensity, low luminous intensity of complexes, and energy level matching Not very good and other problems, to achieve good luminous intensity, prevent fluorescence quenching, and improve spinnability

Active Publication Date: 2015-06-03
湖州信倍连网络科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

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 luminescent nylon and preparation method thereof
  • Organic rare earth europium luminescent nylon and preparation method thereof
  • Organic rare earth europium luminescent nylon and preparation method thereof

Examples

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preparation example Construction

[0034] The invention provides a method for preparing organic rare earth europium luminescent nylon, which comprises the following steps:

[0035] (1) prepare organic rare earth europium complex luminescent material, its chemical formula is C 24 h 16 EuN 4 SF 3 o 2 , the molecular formula is Eu(TTA) 3 DmPPhen, where TTA is: α-thiophene trifluoroformylacetone, DmPPhen is: 2,3-dimethylpyrazino[1,10]phenanthroline, and the structural formula is:

[0036]

[0037] The structural units of the complex are as follows:

[0038]

[0039] (2) Blending the organic rare earth europium complex luminescent material with PA6 (Polyamide 6, polycaprolactam) slices, and then melt-spinning to obtain luminescent nylon.

[0040] Specifically, the preparation method of organic rare earth europium complex luminescent material comprises the following steps:

[0041] (1) Preparation of ligand 2,3-dimethylpyrazino[1,10]phenanthroline:

[0042] a. Put 1,10-phenanthroline and potassium bromi...

Embodiment 1

[0076] Rare earth europium complex Eu(TTA) 3 The preparation process of DmPPhen is as follows:

[0077] 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

[0094] 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:

[0095] Fully mix the nano-scale luminescent material prepared above with the PA6 masterbatch, use a twin-screw extruder to prepare a color masterbatch containing 5% of the organic rare earth complex, and dry it in vacuum at 120° C. for 10 hours to make the water content less than 20 ppm.

[0096] The PA6 slices are transported to a vacuum drum for drying, the set temperature is 120°C, the vacuum degree is 0.095MPa, and the drying time is 16h.

[0097] The dried material is fed into the single-screw extruder at the same time as the color masterbatch with the rare earth luminescent material, and the feeding amount of the color masterbatch is controlled so that the ra...

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Abstract

The invention discloses organic rare earth europium luminescent nylon and a preparation method thereof. The rare earth europium complex Eu(TTA)3DmPPhen luminescent material close to nanoscale is prepared by firstly preparing a phenanthroline neutral ligand and carrying out coordination on the phenanthroline neutral ligand and rare earth Eu (III) in combination with alpha-thenoyltrifluoroacetone and adopting a method of firstly carrying out titration under atmospheric pressure and secondly carrying out reaction under high pressure. The material emits strong pure red light at 615nm in a 10-5mol / L CH2Cl2 solution. The luminescent fiber is prepared by adopting the complex as a luminescent material and carrying out compound melt spinning on the complex and PA6 (polyamide 6). When the content of the rare earth luminescent material in the fiber is 0.08%, the fiber emits stronger pure red light in a 10-5mol / L DMF (dimethyl formamide) solution and the luminescent position is still at 615nm. The luminescent fiber has the advantages of high colour purity and better spinnability.

Description

technical field [0001] The invention belongs to the field of light-emitting materials and textile science, and in particular relates to an organic rare-earth europium light-emitting nylon 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): D01F6/90D01F1/10C09K11/06C07F5/00
Inventor 顾玲袁欢欢顾昕提云崇徐国华
Owner 湖州信倍连网络科技有限公司
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