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Tetraalkoxy phenyl sulpho-diene nickel and preparation method thereof

A technology of tetraalkoxyphenyl thiodiene and thiodiene nickel is applied in the field of near-infrared absorption dye-thiodiene nickel complex and its preparation, and can solve the problem of thiodiene nickel complex lack etc.

Inactive Publication Date: 2010-01-13
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the maximum absorption wavelength λmax of the thiodiene nickel complexes prepared in the prior art is mostly in the range of 700nm to 920nm and 1000nm to 1400nm, while in the range of 920nm to 1000nm, especially the sulfur in the range of 940nm to 980nm Diene nickel complexes are relatively scarce

Method used

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  • Tetraalkoxy phenyl sulpho-diene nickel and preparation method thereof
  • Tetraalkoxy phenyl sulpho-diene nickel and preparation method thereof
  • Tetraalkoxy phenyl sulpho-diene nickel and preparation method thereof

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Embodiment

[0014] First, add 40mL of dichloromethane, 13.86g of anhydrous aluminum chloride, and 20mL of nitrobenzene into a 250mL four-neck flask equipped with a stirring device, a reflux condenser with a calcium chloride drying tube, a thermometer, and a dropping funnel. Under the action of a constant temperature and low temperature bath, control the temperature below 5°C, slowly add 11.5mL of phthalic dimethyl ether, and after a period of time, slowly add oxalic acid chloride solution (3.5mL oxalyl chloride, 18mL dichloromethane, 9mL nitrobenzene) to control The temperature does not exceed 5°C. After the dropwise addition was completed, stirring was continued for 9 hours under the condition that the temperature was lower than 7°C. The reaction solution was dropped into 120 g of crushed ice and kept stirring, and then the resulting liquid was transferred to a 250 mL flask for steam distillation to remove the solvent and unreacted phthalate. The residue in the bottle was cooled, filter...

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Abstract

The invention relates to a tetraalkoxy phenyl sulpho-diene nickel and a preparation method thereof, belonging to the synthesis technology of organic chemistry. A diketone route synthesis method is adopted to prepare tetraalkoxy phenyl substituted sulpho-diene nickel complex; the aim of increasing the maximum absorption wavelength of the sulpho-diene nickel complex can be achieved by utilizing the adjustability of the maximum absorption wavelength of the sulpho-diene nickel complex. Dialkoxy substituted benzene reacts with oxalyl chloride under the catalysis of anhydrous aluminium trichloride to generate corresponding ortho-diketone which then reacts with phosphorus pentasulfide to generate corresponding sulphur phosphide, and finally the obtained sulphur phosphide reacts with nickel chloride water solution to obtain the tetraalkoxy phenyl sulpho-diene nickel. The prepared tetramethoxyl phenyl sulpho-diene nickel C has the maximum absorption wavelength lambda max within the range of 940-980nm in methylbenzene, 1, 2-dichloroethane, N, N-dimethyl formamide (DMF) solution, can be used for preparing near-infrared absorption filter material, and has great practicability.

Description

technical field [0001] The invention relates to an organic chemical synthesis technology, in particular to a near-infrared absorbing dye-thiodiene nickel complex and a preparation method thereof. Background technique [0002] Thiodiene-type metal complexes are a kind of near-infrared absorbing dyes, which have very good light stability and thermal stability, and also have good electrical and magnetic properties. There are many patent documents describing the synthesis and application of such compounds, such as US patent documents with patent numbers 3806462, 3588216, 4593113, 4675423, 4791023 and 4921317 respectively. Thiodiene nickel complexes are one of the important near-infrared absorbers, which can be used to prepare near-infrared absorption filter materials. By introducing groups, its optical properties such as the maximum absorption wavelength can be adjusted, so that the maximum absorption wavelength can move within the near-infrared absorption band of 700nm to 1400...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C09B57/10
Inventor 陈永杰高志博尚洋洋熊兴琼赵玉凯
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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