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Method for preparing luminescent material 8-hydroxyquinoline calcium

A technology of calcium hydroxyquinoline and luminescent material, applied in luminescent materials, chemical instruments and methods, organic chemistry, etc., can solve the problems of complicated steps, long time, and high cost, and achieve easy process control, short reaction time and low cost. Effect

Inactive Publication Date: 2016-03-30
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The purpose of the present invention is to propose a method with high yield, high purity and few steps in view of the disadvantages of low yield, low purity, complicated steps, long time and high cost in the existing method for preparing the luminescent material calcium 8-hydroxyquinolate. The method for preparing 8-hydroxyquinoline calcium with short period, no additional alkali neutralization reagent, simple operation, green environmental protection and low cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Calcium hydroxide in molar ratio: 8-hydroxyquinoline = 1:2, total amount of raw materials: deionized water = 1kg: 50L, 20.330kg (274.42mol) calcium hydroxide and 79.670kg (548.84mol) 8 - Add hydroxyquinoline to the container, add 5000L deionized water to dissolve or disperse evenly;

[0024] 2) Reaction: heating and stirring at 85° C. for 4 hours;

[0025] 3) Cooling and filtering: cooling to room temperature, filtering, and washing with 85°C deionized water for 3 to 5 times;

[0026] 4) Drying: transfer the product to an oven, raise the room temperature to 105° C. and keep it warm for 1 hour, cool to room temperature and discharge to obtain calcium 8-hydroxyquinolate with a purity of 97.42% and a yield of 82.46%.

Embodiment 2

[0028] 1) Calcium hydroxide in molar ratio: 8-hydroxyquinoline = 1:2, total amount of raw materials: deionized water = 1kg: 50L, 20.330kg (274.42mol) calcium hydroxide and 79.670kg (548.84mol) 8 - Add hydroxyquinoline to the container, add 5000L deionized water to dissolve or disperse evenly;

[0029] 2) Reaction: heating and stirring at 90° C. for 4 hours;

[0030] 3) Cooling and filtering: cooling to room temperature, filtering, and washing with 85°C deionized water for 3 to 5 times;

[0031] 4) Drying: transfer the product to an oven, raise the room temperature to 105° C. and keep it warm for 1 hour, cool to room temperature and discharge to obtain 8-hydroxyquinoline calcium with a purity of 98.17%, and the yield is 86.72%.

Embodiment 3

[0033] 1) Calcium hydroxide in molar ratio: 8-hydroxyquinoline = 1:2, total amount of raw materials: deionized water = 1kg: 50L, 20.330kg (274.42mol) calcium hydroxide and 79.670kg (548.84mol) 8 - Add hydroxyquinoline to the container, add 5000L deionized water to dissolve or disperse evenly;

[0034] 2) Reaction: heating and stirring at 95°C for 4 hours;

[0035] 3) Cooling and filtering: cooling to room temperature, filtering, and washing with 85°C deionized water for 3 to 5 times;

[0036] 4) Drying: transfer the product to an oven, raise the room temperature to 105° C. and keep it warm for 1 hour, cool to room temperature and discharge to obtain 8-hydroxyquinoline calcium with a purity of 98.26%, and the yield is 79.27%.

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Abstract

The invention discloses a method for preparing 8-hydroxyquinoline calcium. The method comprises four steps of burdening: adding raw materials into a container at the molar ratio of calcium hydroxide to 8-hydroxyquinoline calcium of 1:2, and adding the raw materials into the deionized water for dissolving or dispersing uniformly at the molar ratio of raw material total amount to deionized water of 1kg:50L; reaction: heating and stirring for 4 hours at the temperature of 80-100DEG C; cooling and filtering: cooling to room temperature, filtering, and washing with the deionized water at 85DEG C for 3-5 times; drying: transforming the product into an oven, raising the room temperature to 105DEG C and keeping temperature for 1h, cooling to room temperature and discharging to obtain the 8-hydroxyquinoline calcium. The method disclosed by the invention can be used for solving the problems that an alkali neutralization reagent is needed to add in the tradition, a series of complex operations such as removal and purification of side products can be omitted at the same time and low yield and purity of products are caused by side products and surplus operations. The method disclosed by the invention has short process, high purity and no need of alkali neutralization reagent, is simple to operate and easy to control, is low in cost and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of organic electroluminescent materials, in particular to a method for preparing 8-hydroxyquinoline calcium by using calcium hydroxide as a raw material without adding an alkali neutralizing agent through a precipitation conversion method. Background technique [0002] Organometallic complex light-emitting materials not only have the advantages of high fluorescence quantum efficiency of organic substances, but also have the advantages of stability of inorganic substances. The preparation method is simple and fast, and they are ideal materials for realizing the commercialization of organic electroluminescent devices. With the deepening of scientific research, more and more organic electroluminescent materials have been reported, among which 8-hydroxyquinoline metal complexes have been widely studied and applied as organic electroluminescent materials with excellent performance. [0003] Alq 3 As a basic mate...

Claims

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Application Information

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IPC IPC(8): C07D215/30C09K11/06
CPCC07D215/30C09K11/06C09K2211/1029
Inventor 吴诗婷万婷钟学明
Owner NANCHANG HANGKONG UNIVERSITY
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