Metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and preparation method thereof

A technology of nonlinear optics and triazoles, applied in organic chemistry methods, chemical instruments and methods, luminescent materials, etc., to achieve the breakthrough effect of laser protection

Active Publication Date: 2019-01-25
JIANGSU UNIV
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  • Description
  • Claims
  • 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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  • Metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and preparation method thereof
  • Metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and preparation method thereof
  • Metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0039] Step 1: Iridium dichloro bridge compound [Ir(ppy) 2 (μ-Cl) 2 ] 2 Synthesis

[0040] Add iridium trichloride hydrate (350mg, 1mmol) and 2-phenylpyridine ligand (0.5ml, 2.5mmol) into the flask, 45mL of ethylene glycol ether and 15mL of water, and seal the flask under vacuum at 135°C Heat to reflux for 24 hours. After cooling to room temperature, vacuum filtration was carried out with a Buchner funnel, and the obtained precipitate was washed with ethanol and petroleum ether to remove reactants and impurities to obtain a goose yellow powdery solid, which was weighed after air drying (395 mg, 32%).

[0041] Step 2: Synthesis of Auxiliary Ligands, Preparing Route Pieces figure 1 (A);

[0042] Add 10.4g (0.1mol) of dicyanopyridine powder into a 250mL flask, then weigh 15g (0.3mol) (85%) of hydrazine hydrate and 10.5g (0.1mol) of hydrazine hydrochloride, add 100ml of ethylene glycol in the flask Reflux the reaction in an oil bath at 130°C for 6 hours with continuous stirr...

Embodiment 2

[0048] Step 1 and step 2 are the same as embodiment 1;

[0049] Step 3: Synthesis of metal iridium complexes

[0050] Get 110mg of the product of step 1 and 52mg of the product obtained in step 2 and add it to a 100ml reaction flask, add 40ml of methylene chloride and 15ml of methanol, and then add 40mg of KPF to it 6 . Nitrogen was passed through the bottle for 15 minutes to avoid light, and then the temperature of the oil bath was raised to 75°C, and the reaction was stirred and refluxed for 24 hours. The reaction solution was cooled, added an appropriate amount of silica gel and spin-dried, then purified by column chromatography (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 subjected to normal temperature diffusion culture with (acetone-n-hexane), and yellow needle-like crystals were obtained after 4 days, and single crystal structure characterization (CCD) w...

Embodiment 3

[0054] Step 1 and step 2 are the same as embodiment 1;

[0055] Step 3: Synthesis of metal iridium complexes

[0056] Get 110mg of the product of step 1 and 52mg of the product obtained in step 2 and add it to a 100ml reaction flask, add 40ml of methylene chloride and 15ml of methanol, and then add 40mg of KPF to it 6 . Nitrogen was passed through the bottle for 15 minutes, and then the temperature of the oil bath was raised to 95°C, and the reaction was stirred and refluxed for 24 hours. The reaction solution was cooled, added an appropriate amount of silica gel and spin-dried, 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 subjected to normal temperature diffusion culture with (acetone-n-hexane), and yellow needle-like crystals were obtained after 4 days, and single crystal structure characterization (CCD) was carried out ...

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Abstract

The invention belongs to the field of a nonlinear optical material, and discloses a metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material and a preparation method thereof. An iridium dichloro bridge compound and an organic auxiliary ligand of 4-amidogen-3,5-bi-(4-pyridine)-1,2,4-triazole are synthesized into a metal iridium complex; then, the metal iridium complex and the graphene oxide are used to be synthesized into the metal iridium-triazole crystal-graphene oxide ternary nonlinear optical material; the metal iridium complex is connected onto the graphene oxide surface in a covalent form. The characteristic combination of the metal iridium complex and a nanometer functional material is realized; a Z-scanning technology shows that the composite material has higher nonlinear absorption response on metal iridium complex monomers.

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 high-tech fields and national defense construction, including polymers, organic and inorganic crystals, composite materials and organometallic compounds, among which graphene oxide has attracted people's attention due to its unique properties. Coordination polymers (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 to self-assemble through intermolecular interactions such as coordination bonds and π-π* stacking interactions. . The diverse selectivity of organic ligands and metal ions (and auxiliary ligands can...

Claims

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Application Information

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Patent Type & Authority Applications(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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