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A kind of preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum

A quinoline aluminum, electronic-grade technology is applied to the preparation field of electronic-grade high-purity 8-hydroxyquinoline aluminum, can solve the problems of small equipment, difficult to achieve large-scale production, low purification efficiency and the like, and achieves high yield, Suitable for mass production, simple operation effect

Active Publication Date: 2022-05-20
NINGBO NATA OPTO ELECTRONICS MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The commonly used method of purifying 8-hydroxyquinoline aluminum is the sublimation method at present, and the equipment of this method is little, and purification efficiency is low, is difficult to realize large-scale production, so be badly in need of a kind of simple and efficient, suitable for large-scale production of electronic grade high-purity 8- The preparation method of aluminum quinolate

Method used

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  • A kind of preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum

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preparation example Construction

[0023] In order to solve the above problems, the invention provides a kind of preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum, comprising the following steps:

[0024] a. Provide an organic solvent A and an organic solvent B with a purity of not less than 99vol%, and the organic solvent A is selected from dichloromethane, chloroform, tetrachloromethane, N, N-dimethylformamide, dimethyl A mixture of one or more of sulfoxides, the organic solvent B is selected from a mixture of one or more of methanol, ethanol, ethylene glycol, acetone, n-hexane, cyclohexane, and isopropanol;

[0025] b. Dissolve the 8-hydroxyquinoline aluminum crude product in the organic solvent A, stir, filter, and collect the filtrate;

[0026] c. Add the filtrate to the organic solvent B, let stand, filter, and collect the precipitate;

[0027] d. Heating and drying the precipitate collected in step c under vacuum conditions, to obtain.

[0028] 8-Hydroxyquinoline aluminum, ...

Embodiment 1

[0053] Embodiment 1 provides a kind of preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum, comprising the following steps:

[0054] a. providing dichloromethane and n-hexane with a purity of 99.99vol%, which are purified by rectification;

[0055] b. Dissolve 10g of crude aluminum 8-hydroxyquinoline in 200mL of dichloromethane, stir at 25°C for 30min, filter to remove insoluble matter, and collect the filtrate;

[0056] c. Add the filtrate dropwise to 500mL of n-hexane at a speed of 0.2mL / s. After the 8-hydroxyquinoline aluminum is precipitated, let stand, filter, and collect the precipitate;

[0057] d. Heat the precipitate collected in step c to 150° C. and dry for 8 hours under a vacuum pressure of 0.1 kPa to obtain.

[0058] The present embodiment obtains 8.9 g of the product, and the yield is 89%.

Embodiment 2

[0060] Embodiment 2 provides a kind of preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum, comprising the following steps:

[0061] a. providing chloroform and ethanol with a purity of 99.99vol%, which are purified by rectification;

[0062] b. Dissolve 10g of crude aluminum 8-hydroxyquinoline in 150mL of chloroform, stir at 50°C for 30min, filter to remove insoluble matter, and collect the filtrate;

[0063] c. Add the filtrate dropwise to 500mL ethanol at a speed of 0.1mL / s, after the 8-hydroxyquinoline aluminum is precipitated, let stand, filter, and collect the precipitate;

[0064] d. Heat the precipitate collected in step c to 200° C. and dry for 6 hours under a vacuum pressure of 0.5 kPa to obtain the obtained product.

[0065] The present embodiment obtains 9.3 g of the product, and the yield is 93%.

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Abstract

The invention discloses a preparation method of electronic grade high-purity 8-hydroxyquinoline aluminum, comprising the following steps: a. providing organic solvent A and organic solvent B with a purity not lower than 99vol%; b. preparing 8-hydroxyquinoline The aluminum crude product is dissolved in the organic solvent A, stirred, filtered, and the filtrate is collected; c. The filtrate is added to the organic solvent B, allowed to stand, filtered, and the precipitate is collected; d. The precipitate collected in step c is heated and dried under vacuum conditions, Instantly. The method is simple in operation, high in production efficiency, easy to obtain reagent raw materials, low in cost, and high in yield, which meets the application requirements in organic electroluminescent materials. Compared with traditional methods, it is more suitable for large-scale production and is suitable for use in the industry. Promote widely.

Description

technical field [0001] The invention relates to a purification method, in particular to a preparation method of electronic-grade high-purity 8-hydroxyquinoline aluminum. Background technique [0002] 8-Hydroxyquinoline aluminum is a metal complex used in organic electroluminescent materials (OLED), and it is also one of the best electron transport materials reported so far. People have carried out a lot of research work on its photoelectric properties and found that 8 -Aluminum hydroxyquinoline has good thermal stability and film-forming properties, and its amorphous film carrier mobility can reach (4.63±5.34)*10 -6 cm 2 ·V -1 ·s -1 , under the excitation of ultraviolet light, the 8-hydroxyquinoline aluminum amorphous powder emits green fluorescent light, and the fluorescent quantum efficiency is as high as 32%, which is a good green light material. Based on the above advantages, people can see the broad application prospects of 8-hydroxyquinoline aluminum in the OLED fi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/30
CPCC07D215/30
Inventor 余绍山陈玲齐国强朱胜恺顾大公毛智彪许从应
Owner NINGBO NATA OPTO ELECTRONICS MATERIAL CO LTD