A kind of method directly preparing pure 8-hydroxyquinolate calcium

Abstract

A kind of method of the present invention directly prepares pure 8-hydroxyquinoline calcium, with calcium oxide and 8-hydroxyquinoline as raw materials, calcium oxide:8-hydroxyquinoline=1:2 according to the molar ratio, the reaction raw materials are added alternately In the ball mill jar; the grinding balls are agate balls, and the mass ratio of the grinding balls to calcium oxide and 8-hydroxyquinoline materials is 10:1 to 20:1. Fill the ball milling jar with nitrogen gas, the volume of which is 3 to 5 times the volume of the ball milling jar, and then start the ball milling. The rotational speed of the ball mill is 200 r / min to 300 r / min, the ball milling time is 70 min to 90 min, and the ball milling reaction temperature is maintained at 90°C to 110°C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydroxyquinoline calcium product with a purity of 98% to 99% and a yield of 97% to 99%. The invention has the advantages of environmental protection, short process flow, high utilization rate of reactants, low production cost and the like.

Description

technical field

[0001] The invention relates to a method for directly preparing pure 8-hydroxyquinoline calcium, in particular to a method for directly preparing pure 8-hydroxyquinoline calcium by using calcium oxide and 8-hydroxyquinoline as reactants by ball milling. The invention specifically belongs to the technical field of metal organic complex preparation. Background technique

[0002] At present, 8-hydroxyquinoline and its derivatives and metal ions (mainly including Al 3+ , Zn 2+ 、Cu 2+ etc.) Formed complex salt-type complexes have become the most eye-catching type of complex luminescent materials in organic light-emitting materials, and the research hotspots focus on aluminum complexes and heavy metal complexes. In order to further improve and enhance the luminescent properties of such complexes, replacing the metal ions in them is a simple and effective way. With the development and deepening of related research, alkaline earth metal elements that are environm...

Examples

Embodiment 1

[0013] According to the molar ratio of calcium oxide: 8-hydroxyquinoline = 1:2, the reaction raw materials were alternately added to a 100 L ball mill jar, a total of 1.500 kg of calcium oxide was added, and a total of 7.765 kg of 8-hydroxyquinoline was added. The grinding balls are agate balls, the mass ratio of the grinding balls to the material (calcium oxide + 8-hydroxyquinoline) is 15:1, and the mass of the agate balls is 138.98 kg. Nitrogen was charged into the ball mill jar, the nitrogen flow rate was 25 L / min, the nitrogen gas flow time was 20 min, and the volume of nitrogen gas charged was 500 L, which was 5 times the volume of the ball mill jar, and then ball milling was started. The rotational speed of the ball mill was 250 r / min, the ball milling time was 80 min, and the ball milling reaction temperature was maintained at 100 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydrox...

Embodiment 2

[0015] Calcium oxide: 8-hydroxyquinoline=1:2 according to the molar ratio, the reaction raw materials are added alternately in the 100 L ball mill jar, calcium oxide adds up to 2.000 kg, 8-hydroxyquinoline adds up to 10.354 grinding balls to be agate balls, grinds The mass ratio of the ball to the material (calcium oxide + 8-hydroxyquinoline) is 10:1, and the mass of the agate ball is 123.54 kg. Nitrogen was filled into the ball mill jar, the nitrogen flow rate was 10 L / min, the nitrogen flow time was 30 min, and the volume of nitrogen gas filled was 300 L, which was three times the volume of the ball mill jar, and then ball milling was started. The rotational speed of the ball mill was 300 r / min, the ball milling time was 70 min, and the ball milling reaction temperature was maintained at 110 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydroxyquinoline calcium product with a purity of 9...

Embodiment 3

[0017] According to the molar ratio of calcium oxide: 8-hydroxyquinoline = 1:2, the reaction raw materials were alternately added to a 100 L ball mill jar, a total of 1.000 kg of calcium oxide was added, and a total of 5.177 kg of 8-hydroxyquinoline was added. The grinding balls are agate balls, the mass ratio of the grinding balls to the material (calcium oxide + 8-hydroxyquinoline) is 20:1, and the mass of the agate balls is 123.54 kg. Fill the ball milling tank with nitrogen, the nitrogen flow rate is 40 L / min, the nitrogen gas flow time is 10 min, and the volume of nitrogen filling is 400 L, which is 4 times the volume of the ball milling tank, and then the ball milling starts. The rotational speed of the ball mill was 200 r / min, the ball milling time was 90 min, and the ball milling reaction temperature was maintained at 90 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydroxyquinolin...

technical field

[0001] The invention relates to a method for directly preparing pure 8-hydroxyquinoline calcium, in particular to a method for directly preparing pure 8-hydroxyquinoline calcium by using calcium oxide and 8-hydroxyquinoline as reactants by ball milling. The invention specifically belongs to the technical field of metal organic complex preparation. Background technique

[0002] At present, 8-hydroxyquinoline and its derivatives and metal ions (mainly including Al 3+ , Zn 2+ 、Cu 2+ etc.) Formed complex salt-type complexes have become the most eye-catching type of complex luminescent materials in organic light-emitting materials, and the research hotspots focus on aluminum complexes and heavy metal complexes. In order to further improve and enhance the luminescent properties of such complexes, replacing the metal ions in them is a simple and effective way. With the development and deepening of related research, alkaline earth metal elements that are environm...

Examples

Embodiment 1

[0013] According to the molar ratio of calcium oxide: 8-hydroxyquinoline = 1:2, the reaction raw materials were alternately added to a 100 L ball mill jar, a total of 1.500 kg of calcium oxide was added, and a total of 7.765 kg of 8-hydroxyquinoline was added. The grinding balls are agate balls, the mass ratio of the grinding balls to the material (calcium oxide + 8-hydroxyquinoline) is 15:1, and the mass of the agate balls is 138.98 kg. Nitrogen was charged into the ball mill jar, the nitrogen flow rate was 25 L / min, the nitrogen gas flow time was 20 min, and the volume of nitrogen gas charged was 500 L, which was 5 times the volume of the ball mill jar, and then ball milling was started. The rotational speed of the ball mill was 250 r / min, the ball milling time was 80 min, and the ball milling reaction temperature was maintained at 100 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydrox...

Embodiment 2

[0015] Calcium oxide: 8-hydroxyquinoline=1:2 according to the molar ratio, the reaction raw materials are added alternately in the 100 L ball mill jar, calcium oxide adds up to 2.000 kg, 8-hydroxyquinoline adds up to 10.354 grinding balls to be agate balls, grinds The mass ratio of the ball to the material (calcium oxide + 8-hydroxyquinoline) is 10:1, and the mass of the agate ball is 123.54 kg. Nitrogen was filled into the ball mill jar, the nitrogen flow rate was 10 L / min, the nitrogen flow time was 30 min, and the volume of nitrogen gas filled was 300 L, which was three times the volume of the ball mill jar, and then ball milling was started. The rotational speed of the ball mill was 300 r / min, the ball milling time was 70 min, and the ball milling reaction temperature was maintained at 110 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydroxyquinoline calcium product with a purity of 9...

Embodiment 3

[0017] According to the molar ratio of calcium oxide: 8-hydroxyquinoline = 1:2, the reaction raw materials were alternately added to a 100 L ball mill jar, a total of 1.000 kg of calcium oxide was added, and a total of 5.177 kg of 8-hydroxyquinoline was added. The grinding balls are agate balls, the mass ratio of the grinding balls to the material (calcium oxide + 8-hydroxyquinoline) is 20:1, and the mass of the agate balls is 123.54 kg. Fill the ball milling tank with nitrogen, the nitrogen flow rate is 40 L / min, the nitrogen gas flow time is 10 min, and the volume of nitrogen filling is 400 L, which is 4 times the volume of the ball milling tank, and then the ball milling starts. The rotational speed of the ball mill was 200 r / min, the ball milling time was 90 min, and the ball milling reaction temperature was maintained at 90 °C. After the ball milling reaction is completed, the material is discharged and cooled to room temperature to obtain a yellow-green 8-hydroxyquinolin...