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A method for directly preparing luminescent material 8-hydroxyquinoline magnesium

A technology of magnesium hydroxyquinoline and luminescent materials, applied in luminescent materials, chemical instruments and methods, organic chemistry, etc., can solve the problems of low product yield, high production cost, and low product purity, and achieve high purity and low production cost. Low, high yield effect

Inactive Publication Date: 2018-03-09
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is aimed at the disadvantages of large waste liquid pollution, low product purity, low product yield and high production cost in the technology of preparing 8-hydroxyquinoline magnesium by liquid phase method, and proposes high atom utilization rate, high product purity and high yield. A new method for preparing pure magnesium 8-hydroxyquinoline with high production cost and low production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] According to mol ratio is magnesium oxide: 8-hydroxyquinoline=1:2.08, 2.000 kg magnesium oxide and 14.983kg 8-hydroxyquinoline of reaction raw material are added in the 1000 L hydrothermal reactor; According to the water consumption of every kilogram of reactant is 15 L, add 254.74 L of distilled water into the hydrothermal reactor; pump air to reduce the vacuum degree of the hydrothermal reactor to 0.1 Pa, stop pumping, heat up to 160 °C under stirring, and the reaction time is 100 min; the reaction is completed , cooled to 85°C, filtered, washed the solid product three times with 85°C hot distilled water; then dried the solid product at 105°C for 60 min, cooled to room temperature, and finally obtained the yellow-green 8-hydroxyquinoline magnesium product with a purity of 98 %, the yield is 94%.

Embodiment 2

[0017] According to mol ratio is magnesium oxide: 8-hydroxyquinoline=1:2.10, 1.500 kg magnesium oxide and 11.345kg 8-hydroxyquinoline of reaction raw material are added in the 1000 L hydrothermal reactor; According to the water consumption of every kilogram of reactant is 20 L, add 256.90 L of distilled water into the hydrothermal reactor; pump air to reduce the vacuum degree of the hydrothermal reactor to 0.1 Pa, stop pumping, heat up to 170 °C under stirring, and the reaction time is 90 min; the reaction is completed , cooled to 90°C, filtered, washed the solid product three times with 90°C hot distilled water; then dried the solid product at 105°C for 60 min, cooled to room temperature, and finally obtained the yellow-green 8-hydroxyquinoline magnesium product with a purity of 99 %, the yield is 92%.

Embodiment 3

[0019] According to mol ratio is magnesium oxide: 8-hydroxyquinoline=1:2.06, 3.000 kg magnesium oxide and 22.258kg 8-hydroxyquinoline of reaction raw material are added in the 1000 L hydrothermal reactor; According to the water consumption of every kilogram of reactant is 10 L, add 252.58 L of distilled water into the hydrothermal reactor; pump air to reduce the vacuum degree of the hydrothermal reactor to 0.1 Pa, stop pumping, heat up to 150 °C under stirring, and the reaction time is 120 min; the reaction is completed , cooled to 80°C, filtered, washed the solid product three times with 80°C hot distilled water; then dried the solid product at 105°C for 60 min, cooled to room temperature, and finally obtained the yellow-green 8-hydroxyquinoline magnesium product with a purity of 97 %, the yield is 95%.

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Abstract

A kind of method of the present invention directly prepares luminescent material 8-hydroxyquinoline magnesium, with magnesium oxide and 8-hydroxyquinoline as raw materials, with water as reaction medium, according to the molar ratio is magnesium oxide:8-hydroxyquinoline=1: 2.06~1:2.10, according to the amount of water per kilogram of reactant is 10L~20L, add the reaction raw materials and distilled water into the hydrothermal reactor. After pumping air to reduce the vacuum degree of the hydrothermal reactor to 0.1Pa, stop pumping, and heat up to 150°C-170°C under stirring, and the reaction time is 90min-110min. After the reaction is complete, cool to 80°C to 90°C, filter, and wash the solid product three times with hot distilled water. Then, the solid product was dried at 105° C. for 60 minutes, and cooled to room temperature; finally, a yellow-green 8-hydroxyquinoline magnesium product was obtained with a purity of 97%-99% and a yield of 92%-95%. The invention has the advantages that the reaction products are 8-hydroxyquinoline magnesium and water, the atom utilization rate is high, the product purity is high, the yield is high, and the production cost is low.

Description

technical field [0001] The invention relates to a method for directly preparing luminescent material 8-hydroxyquinoline magnesium, in particular to a method for directly preparing pure 8-hydroxyquinoline magnesium by hydrothermal method using magnesium oxide and 8-hydroxyquinoline as reactants . The invention specifically belongs to the technical field of metal organic complex preparation. Background technique [0002] The complexes formed by 8-hydroxyquinoline and its derivatives with metal ions are a kind of ideal organic light-emitting materials. At present, more researches are related to aluminum complexes and heavy metal complexes. With the improvement of environmental protection and human safety awareness, the research and development of low-toxic and non-toxic metal ions to replace toxic heavy metal ions in complexes has gradually emerged. As far as the development status is concerned, the most potential metal ions are alkaline earth metal ions, among which magnesiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D215/30C09K11/06
CPCC07D215/30C09K11/06C09K2211/186
Inventor 钟学明
Owner NANCHANG HANGKONG UNIVERSITY