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Method for synthesizing and purifying 8-lithium hydroxyquinoline

A technology of lithium hydroxyquinolate and purification method, which is applied in the field of synthesis and purification of 8-hydroxyquinolate lithium, can solve the problems of high energy consumption and high purification temperature, and achieve simple and safe operation, simple operation, high-efficiency continuous purification The effect of ground purification

Inactive Publication Date: 2019-03-19
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the above three methods, the vacuum sublimation purification method is relatively feasible for industrialization, but the purification temperature of this method is high, the energy consumption is large, and the defects are also extremely obvious.

Method used

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  • Method for synthesizing and purifying 8-lithium hydroxyquinoline
  • Method for synthesizing and purifying 8-lithium hydroxyquinoline
  • Method for synthesizing and purifying 8-lithium hydroxyquinoline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 29.0g (0.20mol) of 8-hydroxyquinoline in methyl tert-butyl ether and configure a solution with a concentration of 95g / L, and dissolve 18.5g (0.44mol) of lithium hydroxide monohydrate in deionized water to prepare 0.5moL / L solution. The 8-hydroxyquinoline solution was mixed with lithium hydroxide aqueous solution, stirred and heated at 60°C for 35 minutes, then allowed to stand for crystallization and filtered. The solid was first purified by recrystallization from 2-methyltetrahydrofuran, and dried to obtain lithium 8-hydroxyquinolate.

[0024] Spread lithium 8-hydroxyquinolate evenly in the sample boat, and turn on the vacuum pump to draw a vacuum. Then set the temperature to 150°C, turn on the heating, preheat the pipeline, and then turn on the cycle condensation. When the temperature is almost reached, set the gas flowmeter to 1mL / min, and open the nitrogen cylinder. In a vacuum environment, the purging of nitrogen makes the newly sublimated product force...

Embodiment 2

[0026] Dissolve 29.0g (0.20mol) of 8-hydroxyquinoline in methyl tert-butyl ether and configure a solution with a concentration of 95g / L, and dissolve 18.5g (0.44mol) of lithium hydroxide monohydrate in deionized water, Prepared into a 0.5moL / L solution. Mix the 8-hydroxyquinoline solution with lithium hydroxide aqueous solution, stir and heat at 60°C for 45 minutes, then stand still for crystallization and filter. The solid was first purified by recrystallization from 2-methyltetrahydrofuran, and dried to obtain lithium 8-hydroxyquinolate.

[0027] The vacuum sublimation purification operation was the same as in Example 1. Yield 73.6%, purity 99.91%.

Embodiment 3

[0029] Dissolve 29.0g (0.20mol) of 8-hydroxyquinoline in methyl tert-butyl ether and configure a solution with a concentration of 95g / L, and dissolve 18.5g (0.44mol) of lithium hydroxide monohydrate in deionized water, Prepared into a 0.5moL / L solution. Mix the 8-hydroxyquinoline solution with lithium hydroxide aqueous solution, stir and heat at 60°C for 60 minutes, then stand for crystallization and filter. The solid was first purified by recrystallization from 2-methyltetrahydrofuran, and dried to obtain lithium 8-hydroxyquinolate.

[0030] The vacuum sublimation purification operation was the same as in Example 1. Yield 71.2%, purity 99.94%.

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Abstract

The invention provides a method for synthesizing and purifying 8-lithium hydroxyquinoline. The method sequentially comprises the steps of mixing an 8-lithium hydroxyquinoline solution with a lithium source water solution, stirring, heating to a certain temperature, reacting for a period of time, standing for crystallization, filtering, carrying out primary purification on a solid by virtue of 2-methyltetrahydrofuran recrystals, drying, and purifying by virtue of a vacuum sublimation device, so as to obtain purifying 8-lithium hydroxyquinoline with a purity over 99.9%.

Description

(1) Technical field [0001] The invention belongs to the field of synthesis of organic and metal coordination compounds, in particular to a synthesis and purification method of 8-hydroxyquinolate lithium. (2) Background technology [0002] Organic electroluminescence (OLE) is a phenomenon in which organic materials are excited to emit light under the action of an external electric field. It has incomparable advantages as a flat panel display and has become another research hotspot in the world today. 8-Hydroxyquinoline metal complexes, as the most mature and widely used organic electroluminescent materials, have good film-forming properties, high quantum efficiency, high glass transition temperature (Tg), and stability Good, good electron transport performance, different metal ions can achieve different colors of luminescence and so on. Among them, 8-hydroxyquinoline lithium has high thermal stability and a melting point of about 365 ° C. At the same time, it has excellent v...

Claims

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Application Information

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IPC IPC(8): C07D215/30
CPCC07D215/30
Inventor 罗书平
Owner 浙江工业大学上虞研究院有限公司
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