Process for producing sulfhydryl functionalized rare earth-macromolecule composite luminescent material

A technology of polymer materials and luminescent materials, which is applied in the field of preparation of mercapto-functionalized rare earth-polymer composite luminescent materials, can solve problems such as uneven distribution of rare earth complexes, phase separation between two phases, and easy agglomeration, so as to achieve easy production of large Large-sized display panel, light and thin quality, and uniform particle size distribution

Inactive Publication Date: 2009-05-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the hybrid material prepared by the above method is connected by weak interaction force between the rare earth complex and the inorganic matrix, so there are problems such as uneven distribution of the rare earth complex and easy agglomeration, and phase separation between the two phases.

Method used

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  • Process for producing sulfhydryl functionalized rare earth-macromolecule composite luminescent material
  • Process for producing sulfhydryl functionalized rare earth-macromolecule composite luminescent material

Examples

Experimental program
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Effect test

Embodiment 1

[0031]Dissolve 1 mol of o-mercaptobenzoic acid in 20L of absolute ethanol, add 1 mol of triethoxysilyl isocyanate propyl isocyanate in absolute ethanol, under the protection of nitrogen atmosphere, reflux at 65°C for 12 hours, and then cool. The solvent was distilled off under reduced pressure. The oily organic bridge precursor of gained is dissolved with dehydrated alcohol, simultaneously 3L polyvinylpyridine is dissolved in 15L anhydrous acetone, it is all added in the three-necked flask, then to be dissolved with mercaptobenzoic acid bridge precursor, polyvinylpyridine Add 1359 g of terbium nitrate to the ethanol solution of vinylpyridine, stir for 2 hours at a temperature of 20° C., then add tetraethyl orthosilicate and deionized water dropwise to adjust the pH to 6. The molar ratio of mercaptobenzoic acid, vinylpyridine, rare earth nitrate, tetraethyl orthosilicate and deionized water is 3:1:1:6:12. The whole solution was stirred at 25°C for 6 hours to obtain a solid gel...

Embodiment 2

[0035] Dissolve 1mol of p-methyl-o-mercaptobenzoic acid in 15L of anhydrous tetrahydrofuran, add dropwise a tetrahydrofuran solution containing 1mol of 3-chloropropyltriethoxysilane, under the protection of a nitrogen atmosphere, reflux at 60°C for 8 hours, and then cool. The solvent was distilled off under reduced pressure. The obtained oily organic bridge precursor was dissolved in absolute ethanol, and 3L of polyvinylpyridine was dissolved in 15L of anhydrous nitrogen, and nitrogen dimethylformamide was added to the three-necked flask, and then dissolved with mercapto Add 1359g of terbium nitrate to the ethanol solution of polyvinylpyridine, the precursor of the benzoic acid bridge, and stir for 2 hours at a temperature of 25°C, then dropwise add tetraethyl orthosilicate and deionized water to adjust the pH to 6. The molar ratio of mercaptobenzoic acid, vinylpyridine, rare earth nitrate, tetraethyl orthosilicate and deionized water is 3:1:1:6:12. The whole solution was sti...

Embodiment 3

[0037] Dissolve 1 mol of o-mercaptobenzoic acid in 20L of anhydrous pyridine, add dropwise the pyridine solution containing 1 mol of aminopropyltriethoxysilane, under the protection of nitrogen atmosphere, reflux at 100°C for 15 hours, then cool and distill off under reduced pressure solvent. The resulting oily organic bridge precursor was dissolved in absolute ethanol, and 3L of polymethyl methacrylate was dissolved in 15L of anhydrous acetone. Body, polymethyl methacrylate ethanol solution, add 1359g terbium nitrate, stir for 2 hours at a temperature of 20°C, then add tetraethyl orthosilicate and deionized water dropwise to adjust the pH value to 6. The molar ratio of mercaptobenzoic acid, methyl methacrylate, rare earth nitrate, tetraethyl orthosilicate and deionized water is 3:1:1:6:12. The whole solution was stirred at 25°C for 6 hours to obtain a solid gel. The obtained solid gel was transferred to an oven for aging treatment, the temperature was controlled at 60° C., ...

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Abstract

The invention belongs to the technical field of luminescent macromolecular composite material, and particularly relates to a method for preparing a sulfhydryl functional rare earth-macromolecular composite luminescent material. In the method, firstly, by adopting an organic synthesis method, aromatic organic micro molecules are grafted in an inorganic silica skeleton to obtain organic bridge precursor; the organic bridge precursor, polymers and rare earth ions are further combined to obtain the rare earth macromolecular material by chemical action; at last, by the sol-gel method, all obtained materials are subjected to polyreaction to obtain dried gel, so that the organic macromolecular polymers with long carbon chains are embedded in silica network substrate by covalent bond; and the dried gel is subjected to dry ageing to obtain the macromolecular composite material with stable chemical and thermodynamic performances, smooth surface appearance and special luminescence emission. The method has the advantages of simple preparation process, mild experimental conditions, strong operability, good reproductivity, low cost, stable quality of obtained products and order appearance, and the sizes of crystal grains can be controlled in the range of micron and nanometer.

Description

technical field [0001] The invention belongs to the technical field of luminescent polymer composite materials, and in particular relates to a preparation method of a mercapto functionalized rare earth-polymer composite luminescent material. Background technique [0002] The rapid development of today's society has made it extremely urgent to discover the functional compounding, performance complementation and optimization of various materials, and to prepare composite materials with excellent performance. Therefore, as soon as the organic-inorganic hybrid system appeared, it immediately attracted great attention from scientists. All countries in the world have invested a lot of manpower, material resources and financial resources to conduct in-depth and meticulous research on this material. Generally speaking, hybrid materials have the following characteristics: inorganic substances and polymers can be combined at the molecular level or nanometer size, and have transparent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C08L83/02C08L39/08C08L33/12C08L33/02C08L35/00
Inventor 闫冰盛凯
Owner TONGJI UNIV
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