A kind of metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and its preparation method

A technology of nonlinear optics and triazoles, applied in organic chemistry methods, chemical instruments and methods, luminescent materials, etc., to achieve good nonlinear optical absorption effects

Active Publication Date: 2021-02-12
JIANGSU UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Trying to combine two kinds of materials with excellent nonlinear optical properties to obtain functional materials with more outstanding optical properties has become a new research idea of ​​the present invention. At present, metal iridium-triazole crystals-graphene oxide ternary composite materials have not yet been developed. see related reports

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  • A kind of metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and its preparation method
  • A kind of metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and its preparation method
  • A kind of metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1: Iridium dichloro bridged compound [Ir(ppy) 2 (μ-Cl)] 2 Synthesis

[0039] Iridium trichloride hydrate (350mg, 1mmol) and 2-phenylpyridine ligand (0.5ml, 2.5mmol), 45mL of ethylene glycol ether and 15mL of water were added to the flask, the flask was sealed and evacuated under nitrogen protection at 135°C Heat to reflux for 24 hours. Cooled to room temperature, vacuum filtered with a cloth funnel, the obtained precipitate was washed with ethanol and petroleum ether to remove reactants and impurities to obtain a light yellow powdery solid, which was naturally dried and weighed (395 mg, 32%).

[0040] Step 2: Synthesis of Auxiliary Ligands, Preparation of Routes figure 1 (A);

[0041] Add 10.4g (0.1mol) of dicyanopyridine powder to a 250mL flask, weigh 15g (0.3mol) (85%) of hydrazine hydrate and 10.5g (0.1mol) of hydrazine hydrochloride, add 100ml of ethylene glycol to the flask The reaction was carried out under reflux in an oil bath at 130° C. for 6 h with c...

Embodiment 2

[0047] Step 1 and step 2 are the same as in Example 1;

[0048] Step 3: Synthesis of Metal Iridium Complexes

[0049] Take 110mg of the product in step 1 and 52mg of the product obtained in step 2 and add it to a 100ml reaction flask, and add 40ml of dichloromethane and 15ml of methanol, and then add 40mg of KPF to it 6 . Nitrogen was passed through the bottle for 15 min and protected from light, the oil bath was heated to 75° C., and the reaction was stirred and refluxed for 24 h. The reaction solution was cooled and an appropriate amount of silica gel was spin-dried, followed by column chromatography purification (dichloromethane-ethanol, two bands were collected), and spin-dried to obtain 74 mg of metal iridium complex solid. The obtained metal iridium complex solid was cultured at room temperature with (acetone-n-hexane), and after 4 days, yellow needle-like crystals were obtained and single crystal structure characterization (CCD) was performed to confirm that the obtai...

Embodiment 3

[0053] Step 1 and step 2 are the same as in Example 1;

[0054] Step 3: Synthesis of Metal Iridium Complexes

[0055] Take 110mg of the product in step 1 and 52mg of the product obtained in step 2 and add it to a 100ml reaction flask, and add 40ml of dichloromethane and 15ml of methanol, and then add 40mg of KPF to it 6 . Nitrogen was passed through the bottle for 15 min, and then the oil bath was heated to 95 °C, and the reaction was stirred and refluxed for 24 h. The reaction solution was cooled and an appropriate amount of silica gel was spin-dried, and then purified by column chromatography (dichloromethane-ethanol, two bands were collected), and spin-dried to obtain 79 mg of metal iridium complex solid. The obtained metal iridium complex solid was cultured at room temperature with (acetone-n-hexane), and after 4 days, yellow needle-like crystals were obtained and single crystal structure characterization (CCD) was performed to confirm that the obtained complex was metal...

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Abstract

The invention belongs to the field of nonlinear optical materials, and discloses a metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and a preparation method thereof. The present invention synthesizes metal iridium complexes with iridium dichloro bridge compound and organic auxiliary ligand 4-amino-3,5-bis-(4-pyridine)-1,2,4-triazole, and then utilizes metal iridium organic coordination compound and graphene oxide to synthesize metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material, and the metal iridium complex is covalently connected on the surface of graphene oxide. The invention realizes the combination of properties of the metal-organic complex and the nano-functional material, and Z-scan technology shows that the composite material has a stronger nonlinear absorption response than the metal iridium complex monomer.

Description

technical field [0001] The invention belongs to the field of nonlinear optical materials, in particular to a metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and a preparation method thereof. Background technique [0002] Nonlinear optical functional materials are important basic materials in the field of high science and technology and national defense construction. They include polymers, organic-inorganic crystals, composite materials and organometallic compounds. Among them, graphene oxide has attracted people's attention due to its unique properties. coordination polymer (CP) S ) is a crystalline material with a zero-dimensional or even multi-dimensional network structure formed by organic ligands connecting metal ions or metal clusters under appropriate conditions through coordination bonds, π-π* stacking and other intermolecular interactions. . The diverse selectivity of organic ligands and metal ions (auxiliary ligands can also be add...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00C09K11/06
CPCC07B2200/13C07F15/0033C09K11/06C09K2211/185
Inventor 张弛钱军聂谦英李璐
Owner JIANGSU UNIV
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