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A cationic metal complex iridium-benzophenanthroline crystal material and its preparation method and application

A technology of metal complexes and benzohydrophenanthroline, applied in luminescent materials, indium organic compounds, organic chemical methods, etc., to achieve good thermal stability and solubility, low transmittance, and reduce the degree of conjugation

Active Publication Date: 2022-07-22
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the deficiency that nonlinear optical materials in the prior art cannot meet the existing needs due to their solubility and transmittance problems, the invention provides a cationic metal complex iridium-benzophenanthroline crystal material and its preparation method and application

Method used

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  • A cationic metal complex iridium-benzophenanthroline crystal material and its preparation method and application
  • A cationic metal complex iridium-benzophenanthroline crystal material and its preparation method and application
  • A cationic metal complex iridium-benzophenanthroline crystal material and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0037] (1) Iridium dichloro bridge compound [Ir(ppz) 2 ( μ -Cl) 2 ] 2 Synthesis:

[0038] Add 350 mg (1 mmol) of hydrated iridium trichloride, 0.288 mL (2.3 mmol) of 1-phenylpyrazole ligand, 24 mL of ethylene glycol ether and 8 mL of water to the reaction flask, under nitrogen protection at 135°C Condensation was refluxed for 24 hours, and the degree of reaction progress was monitored by TLC during the reaction. After the reaction was completed, the solution was cooled to room temperature and filtered with a small Buchner funnel. The resulting precipitate was washed with ethanol and petroleum ether to remove the reaction raw materials and by-products, followed by CH 2 Cl 2 and H 2O was extracted for further purification, and finally the organic phase was spin-dried to obtain 295 mg of pale yellow solid [Ir(ppz) 2 ( μ -Cl) 2 ] 2 (57.2%).

[0039] (2) Synthesis of auxiliary ligand 6,7-dihydrodibenzo-1,10-phenanthroline:

[0040] figure 1 A is the synthetic route o...

Embodiment 2

[0052] Step (1) and step (2) are the same as in Example 1, and other steps are as follows:

[0053] Step 3. Synthesis of iridium-benzophenanthroline:

[0054] In a 50 ml reaction flask, add 100 mg of 6,7-dihydrodibenzo-1,10-phenanthroline and 183 mg of iridium dimer, add 15 mL of dichloromethane and 10 mL of methanol, and finally add 70 mg potassium hexafluorophosphate, pass nitrogen into the bottle for 30 minutes for protection, in an oxygen-free environment protected from light, stir and reflux in an oil bath at 85 °C for 24 hours, add silica gel to the reaction solution and spin dry, and finally separate by column chromatography, spin dry, Iridium-benzophenanthroline was obtained as a solid (73 mg).

[0055] Step 4. Crystal room temperature diffusion culture of iridium-benzophenanthroline:

[0056] According to the ratio of metal iridium complex solid: dichloromethane: buffer layer: n-hexane = 1 mmol: 1 mL: 0.6 ml: 3 mL, the iridium-benzophenanthroline synthesized in step...

Embodiment 3

[0060] Step 1 and step 2 are the same as in embodiment 1, and other steps are as follows:

[0061] Step 3. Synthesis of iridium-benzophenanthroline:

[0062] In a 50 ml reaction flask, add 100 mg of 6,7-dihydrodibenzo-1,10-phenanthroline and 183 mg of iridium dimer, then add 10 mL of dichloromethane and 10 mL of methanol, and finally add 70 mg of hexamethylene Potassium fluorophosphate, pass nitrogen into the bottle for 30 minutes for protection, in an oxygen-free environment protected from light, stir and reflux in an oil bath at 85°C for 24 hours, add silica gel to the reaction solution and spin dry, and finally separate by column chromatography and spin dry to obtain 72 mg iridium-benzophenanthroline solid.

[0063] Step 4. Crystal room temperature diffusion culture of iridium-benzophenanthroline:

[0064] According to the ratio of metal iridium complex solid: dichloromethane: buffer layer: n-hexane = 1 mmol: 1 mL: 0.6 ml: 3 mL, the iridium-benzophenanthroline synthesized...

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Abstract

The invention belongs to the fields of optical limiting materials and laser protection, and relates to a cationic metal complex iridium-benzophenanthroline crystal material and a preparation method and application thereof; The azolyl metal iridium dimer is coordinated with 6,7-dihydrodibenzo-1,10-phenanthroline to form a metal-organic complex, and then the final crystal material is obtained by the normal temperature diffusion method, and the crystal material has excellent The fluorescence emission and nonlinear absorption properties of the ionomers are excellent, and the transmittance can reach 0.526 under laser irradiation with a wavelength of 532 nm and a frequency of 4 ns.

Description

technical field [0001] The invention belongs to the field of optical limiting materials and laser protection, in particular to a cationic metal complex iridium-benzophenanthroline crystal material and a preparation method and application thereof. Background technique [0002] In recent years, organic light-emitting diodes (OLEDs) have received extensive attention due to their promising applications in flat-panel displays and solid-state lighting. Among the many luminescent materials used to prepare OLEDs, Ir(III)-containing metal complexes have become the most studied phosphorescent materials due to their high quantum efficiency, short triplet lifetime, and good photothermal stability. At present, the Ir(III)-containing metal complexes reported at home and abroad are all constructed by a two-step method. First, the dinuclear Ir(III) dichloro-bridged intermediate was synthesized, and then by introducing auxiliary ligands, Ir(III) metal complexes with different structures and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00C09K11/06
CPCC07F15/0033C09K11/06C07B2200/13C09K2211/185C09K2211/1044C09K2211/1007
Inventor 钱军谭倩李璐
Owner JIANGSU UNIV
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