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Method for directly preparing light-emitting material 8-hydroxyquinoline copper

A technology of copper hydroxyquinoline and luminescent materials, applied in luminescent materials, chemical instruments and methods, organic chemistry and other directions, can solve the problems of short process, low cost and high cost, and achieve low production cost, high utilization rate of raw materials, and high productivity. high rate effect

Inactive Publication Date: 2015-07-01
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] The purpose of the present invention is to propose a direct preparation of luminescent materials with high yield, short process and low cost in view of the shortcomings of low yield, long steps and high cost in the existing industrialized method for preparing luminescent material copper 8-hydroxyquinoline 8-hydroxyquinoline copper method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] First, according to the molar ratio of copper formate tetrahydrate / 8-quinolinol=1:2, 262.39 kg of copper formate tetrahydrate and 337.61 kg of 8-quinolinol were sequentially added to the mixer and mixed evenly. Transfer 600 kg of evenly mixed reaction raw materials to a 1000 L reactor. In the vacuum reactor, pump air to reduce the vacuum to 0.1 Pa, then raise the temperature to 80°C-100°C at a heating rate of 1°C / min, and maintain the vacuum The temperature is 0.1 Pa, and the reaction is held for 75 min. After the reaction is completed, cool to room temperature and discharge. Copper 8-hydroxyquinolate with a purity of 99% was obtained with a yield of 98%. The formic acid produced in the vacuum hot melting reaction is recovered by condensation.

Embodiment 2

[0032] First, according to the molar ratio of copper formate tetrahydrate / 8-quinolinol=1:2, 262.39 kg of copper formate tetrahydrate and 337.61 kg of 8-quinolinol were sequentially added to the mixer and mixed evenly. Transfer 600 kg of evenly mixed reaction raw materials to a 1000 L reactor. In the vacuum reactor, pump air to reduce the vacuum to 0.1 Pa, then raise the temperature to 80°C-100°C at a heating rate of 1°C / min, and maintain the vacuum The temperature was 0.1 Pa, and the reaction was held for 90 min. After the reaction is completed, cool to room temperature and discharge. Copper 8-hydroxyquinolate with a purity of 98% was obtained with a yield of 99%. The formic acid produced in the vacuum hot melting reaction is recovered by condensation.

Embodiment 3

[0034] First, according to the molar ratio of copper formate tetrahydrate / 8-quinolinol=1:2, 262.39 kg of copper formate tetrahydrate and 337.61 kg of 8-quinolinol were sequentially added to the mixer and mixed evenly. Transfer 600 kg of evenly mixed reaction raw materials to a 1000 L reactor. In the vacuum reactor, pump air to reduce the vacuum to 0.1 Pa, then raise the temperature to 80°C-100°C at a heating rate of 1°C / min, and maintain the vacuum The temperature was 0.1 Pa, and the reaction was held for 60 min. After the reaction is completed, cool to room temperature and discharge. Copper 8-hydroxyquinolate with a purity of 97% and a yield of 100% was obtained. The formic acid produced in the vacuum hot melting reaction is recovered by condensation.

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Abstract

The invention discloses a method for directly preparing a light-emitting material 8-hydroxyquinoline copper. According to the invention, tetrahydrate copper formate and 8-hydroxyquinoline are adopted as reaction raw materials, and 8-hydroxyquinoline copper is prepared with a vacuum hot-melt method. The method comprises the following specific steps: the raw materials are added into a mixer according to a molar ratio that tetrahydrate copper formate to 8-hydroxyquinoline is 1:2, and the raw materials are well mixed; the well mixed mixture of the reaction raw materials is transferred into a vacuum reaction kettle; the reaction kettle is pumped until a vacuum degree is reduced to 0.1Pa, and the temperature in the reaction kettle is increased to 80-100 DEG C with a heating speed of 1 DEG C / min; the vacuum degree is maintained at 0.1Pa, and a reaction is carried out for 60-90min under a maintained temperature; and when the reaction is finished, an obtained product is cooled to room temperature and is fetched. With the method, 8-hydroxyquinoline copper with purity of 97-99% is obtained, and the yield is 98-100%. The method provided by the invention has the advantages of simplicity in operation, high raw material utilization rate, short process, high yield, no waste liquid discharge, low production cost, and the like.

Description

technical field [0001] The invention relates to a method for directly preparing copper 8-hydroxyquinolate as a luminescent material, in particular to a method for directly preparing copper 8-hydroxyquinolate by using copper formate tetrahydrate as a main raw material through a vacuum hot-melt method. The invention belongs to the technical field of organic electroluminescent materials. Background technique [0002] Copper 8-hydroxyquinoline with a purity higher than 95% has the advantages of good film-forming properties, high quantum efficiency, high glass transition temperature, and good stability. It is one of the modern organic electroluminescent materials that are widely used and attract much attention. . [0003] The existing methods for preparing copper 8-hydroxyquinoline mainly include liquid-phase method and solid-phase method. Liquid-phase methods include liquid-phase precipitation and evaporative crystallization. At present, the industrial preparation of the lumi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/30C09K11/06
CPCC07D215/30
Inventor 钟学明谢宇华莉
Owner NANCHANG HANGKONG UNIVERSITY
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