Organic luminous material and preparation method thereof

Abstract

The invention provides an organic luminous material and a preparation method thereof, and relates to an organic silicon polymer. Raw materials of the organic luminous material comprise metallic organic substance and polycarbosilane. The preparation method comprises the following steps of: putting polydimethylsiloxane into a reaction kettle, heating the polydimethylsiloxane under the protection ofargon, inflating the argon to the reaction kettle, adding n-hexane into the reaction kettle to dissolve the product after the temperature in the reaction kettle is naturally cooled to room temperature, filtering the product, removing the n-hexane in vacuum to obtain the polycarbosilane, soaking the ground polycarbosilane into ethanol, flushing the insoluble substances by using the ethanol and then drying the insoluble substances in vacuum; and pouring the polycarbosilane powder and the metallic organic substance powder into a three-necked bottle, heating the mixed powder to between 150 and 160 DEG C under the protective atmosphere of argon, preserving the heat for 1 to 1.5 hours, heating the mixed powder to between 260 and 270 DEG C, preserving the heat for 1 to 1.5 hours, dissolving the product by using the dry n-hexane after the reaction is finished and the product is cooled, filtering the product to remove the insoluble substances, and finally distilling the product with reduced pressure to obtain the powdery solid organic luminous material.

Description

technical field

[0001] The present invention relates to an organosilicon polymer, in particular to a blue light-emitting material prepared by the synthesis reaction of a metal organic compound and polycarbosilane and a preparation method thereof. The material has blue-violet light emission in the near-ultraviolet band, and the emission peak is located at 430nm about. Background technique

[0002] Organic fluorescence and its corresponding research began in the 1960s, when many electroluminescent phenomena of organic materials composed of hosts with conjugated structures and activators with conjugated structures were reported. The hosts include naphthalene, Anthracene, phenanthrene, tetracene, perylene, benzoperylene, etc., and activators include anthracene, tetracene, pentacene, etc., but due to the high driving voltage required at that time, it did not attract widespread attention.

[0003] In 1987, Tang et al. from Eastern Kodak Company invented a sandwich structure devic...

Examples

Embodiment 1

[0037] 1) Put 50g of polydimethylsiloxane in a closed 300ml reaction kettle, quickly heat up to 300°C under the protection of argon, vacuumize and keep it for 2 hours, then fill it with argon at 101KPa, and then heat up at a rate of 1°C / min The temperature was raised to 390°C for 3 hours. After the reaction was completed, after the temperature in the reactor naturally dropped to room temperature, n-hexane was added to dissolve the product, filtered, and the n-hexane was removed in a vacuum.

[0038] 2) The product in step 1) was ground and soaked in absolute ethanol, stirred for 12 hours, and the filtered product was rinsed with absolute ethanol three times and then dried in a vacuum atmosphere at 60° C. to obtain a light yellow powder.

[0039] 3) Take 10g of the product in step 2), grind it into powder and mix it with 1g of dysprosium acetylacetonate Dy(AcAc) 3 The powder was mixed evenly and placed at the bottom of a 100ml three-neck bottle. After the whole system was evac...

Embodiment 2

[0042] 1) Put 50g of polydimethylsiloxane in a closed 300ml reaction kettle, raise the temperature to 300°C under the protection of argon, vacuumize and keep it for 2h, then fill it with argon at 103KPa, and then increase the temperature at a rate of 2°C / min Raise the temperature to 390°C for 3h. After the reaction was completed, after the temperature in the reactor naturally dropped to room temperature, n-hexane was added to dissolve the product, filtered, and the n-hexane was removed in a vacuum.

[0043] 2) The product in step 1) was ground and soaked in absolute ethanol, stirred for 12 hours, and the filtered product was rinsed with absolute ethanol three times and then dried in a vacuum atmosphere at 60° C. to obtain a light yellow powder.

[0044] 3) Take 10 g of the product in step 2), grind it into powder and mix it with 0.5 g of aluminum acetylacetonate Al(AcAc) 3 Mix the powder evenly and place it at the bottom of a 100ml three-neck bottle. After the whole system is...

technical field

[0001] The present invention relates to an organosilicon polymer, in particular to a blue light-emitting material prepared by the synthesis reaction of a metal organic compound and polycarbosilane and a preparation method thereof. The material has blue-violet light emission in the near-ultraviolet band, and the emission peak is located at 430nm about. Background technique

[0002] Organic fluorescence and its corresponding research began in the 1960s, when many electroluminescent phenomena of organic materials composed of hosts with conjugated structures and activators with conjugated structures were reported. The hosts include naphthalene, Anthracene, phenanthrene, tetracene, perylene, benzoperylene, etc., and activators include anthracene, tetracene, pentacene, etc., but due to the high driving voltage required at that time, it did not attract widespread attention.

[0003] In 1987, Tang et al. from Eastern Kodak Company invented a sandwich structure devic...

Examples

Embodiment 1

[0037] 1) Put 50g of polydimethylsiloxane in a closed 300ml reaction kettle, quickly heat up to 300°C under the protection of argon, vacuumize and keep it for 2 hours, then fill it with argon at 101KPa, and then heat up at a rate of 1°C / min The temperature was raised to 390°C for 3 hours. After the reaction was completed, after the temperature in the reactor naturally dropped to room temperature, n-hexane was added to dissolve the product, filtered, and the n-hexane was removed in a vacuum.

[0038] 2) The product in step 1) was ground and soaked in absolute ethanol, stirred for 12 hours, and the filtered product was rinsed with absolute ethanol three times and then dried in a vacuum atmosphere at 60° C. to obtain a light yellow powder.

[0039] 3) Take 10g of the product in step 2), grind it into powder and mix it with 1g of dysprosium acetylacetonate Dy(AcAc) 3 The powder was mixed evenly and placed at the bottom of a 100ml three-neck bottle. After the whole system was evac...

Embodiment 2

[0042] 1) Put 50g of polydimethylsiloxane in a closed 300ml reaction kettle, raise the temperature to 300°C under the protection of argon, vacuumize and keep it for 2h, then fill it with argon at 103KPa, and then increase the temperature at a rate of 2°C / min Raise the temperature to 390°C for 3h. After the reaction was completed, after the temperature in the reactor naturally dropped to room temperature, n-hexane was added to dissolve the product, filtered, and the n-hexane was removed in a vacuum.

[0043] 2) The product in step 1) was ground and soaked in absolute ethanol, stirred for 12 hours, and the filtered product was rinsed with absolute ethanol three times and then dried in a vacuum atmosphere at 60° C. to obtain a light yellow powder.

[0044] 3) Take 10 g of the product in step 2), grind it into powder and mix it with 0.5 g of aluminum acetylacetonate Al(AcAc) 3 Mix the powder evenly and place it at the bottom of a 100ml three-neck bottle. After the whole system is...

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