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VOC fluorescent sensing material based on cuprous complexes

A technology of fluorescent sensing and complexes, applied in luminescent materials, luminescent coatings, fluorescence/phosphorescence, etc., can solve the problems of high price, ignoring the actual sensing and detection quantification, low cost, etc., and achieve low production cost, cheap purification, inhibition The effect of nonradiative attenuation

Active Publication Date: 2019-06-14
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as mentioned in the article, current researchers in this field usually only study the molecular mechanism of this phenomenon, while ignoring the application requirements such as quantitative and low cost of actual sensing and detection.
In particular, it needs to be pointed out that the platinum and gold used in the reported complexes are expensive, and to meet the low-cost requirements of the application, it is necessary to start with ordinary metals

Method used

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  • VOC fluorescent sensing material based on cuprous complexes
  • VOC fluorescent sensing material based on cuprous complexes
  • VOC fluorescent sensing material based on cuprous complexes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of a large number of luminescent complex material Cu(Xantphos)I crystal powder samples: Weigh 0.037g (0.1mmol) of Cu(CH 3 EN) 4 PF 6 , 0.058g (0.1mmol) of Xantphos were dissolved in 5mL of dichloromethane and mixed, stirred to fully undergo a coordination reaction; then weighed 0.017g (0.1mmol) of KI and dissolved it in 5mL of acetonitrile Then slowly add to the above reaction solution; raise the temperature to start reflux, and maintain the reflux state for 1 hour, then transfer to gradually reduced pressure rotary evaporation, after complete evaporation, add water and ethanol to wash in sequence, and the light yellow crystal powder obtained after drying is the product (see attached image 3 ), the yield was 94% (calculated as Cu). Spectral tests found that the material strongly absorbs ultraviolet light (see attached Figure 4 ), and can emit strong fluorescence (see attached Figure 5 ).

Embodiment 2

[0044] Synthesis of single crystal of luminescent complex material Cu(Xantphos)I: Weigh 0.037g (0.1mmol) of Cu(CH 3 EN) 4 PF 6 , 0.058g (0.1mmol) of Xantphos, 0.017g (0.1mmol) of KI, were dissolved in 3mL of dichloromethane, 2mL of dichloromethane and 5mL of acetonitrile; Cu(CH 3 EN) 4 PF 6 Mix and react with Xantphos solution, stir to make the coordination reaction fully occur, and obtain a light yellow clear solution; after filtering, cover the upper layer of the solution with acetonitrile solution of KI to make it slowly diffuse and react; after standing for a few days, there will be light yellow block crystals Precipitate. Select a light yellow block crystal with a size of 0.26mm*0.20mm*0.16mm for X-ray single crystal structure test. Single crystal structure analysis results, the molecular structure diagram of the compound is shown in the attached figure 1 , and its unit cell packing structure is shown in the attached figure 2 .

Embodiment 3

[0046] Preparation of fluorescent sensing film and its atmosphere response: Weigh 0.1g of PMMA (polymethyl methacrylate, glass transition temperature: 105°C) to completely dissolve it in 2mL of dichloromethane, and the solution is colorless, clear and transparent. Weigh 0.01g of the complex Cu(Xantphos)I, dissolve it in 2mL of dichloromethane, and remove the insoluble matter after thorough stirring. The complex solution was slowly added to the PMMA solution, and the solution was light yellow and clear. Spin-coat (1200rad / min) on a clean quartz plate and dry (60°C, 30min) to obtain a fluorescent sensing film sample. The sensing film sample is placed in a VOC atmosphere, and the fluorescence spectrum is tested after a certain period of time. The test found that the sensing film sample also has a certain fluorescence response performance to the vapors of DMF, triethylamine, methanol, n-butanol, acetonitrile, etc. (see attached Figure 7 ). In particular, the test found that th...

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Abstract

The invention discloses a VOC fluorescent sensing material based on cuprous complexes, a preparation method of the VOC fluorescent sensing material and VOC fluorescent sensing application. A luminouscomplex is prepared by complexing univalent copper salts and ligands; the molecular structure is Cu(Xantphos)I; in the formula, the Xantphos is an electrically neutral diphosphine ligand of 4,5-bis(diphenylphospheno)-9,9-dimethylxanthene; I is a halogen iodide ligand. The complex has the advantages of easy purification of small molecules, and also has high thermal stability. The material is obtained by direct mixing and reaction on the CuI and the ligand acetonitrile solution and dichloromethane solution. The complex has the advantages that the process is simple and convenient; the equipment is simple; the raw materials can be easily obtained; the cost is low, and the like. The material can be used as the VOC fluorescent sensing material, and has the good selective fluorescent response tomethylamine steam.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, to the field of photoluminescent materials, in particular to the field of fluorescent sensing materials. Background technique [0002] Volatile Organic Compounds (Volatile Organic Compound, abbreviated as VOC) generally refer to organic compounds with relatively high saturated vapor pressure at room temperature. In my country, VOC refers to all organic compounds with a saturated vapor pressure exceeding 70Pa at room temperature and a boiling point below 260°C at normal pressure, including hydrocarbons, halogenated hydrocarbons, aldehydes, ketones, organic amines, mercaptans, Low-boiling polycyclic aromatic hydrocarbons, etc. With the development of industry, a large amount of petrochemical resources are consumed to produce emissions; changes in construction and decoration materials, the wide use of various new building materials and interior decoration materials; and a large number ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655C09K11/06C09D133/12C09D5/22G01N21/64
Inventor 朱秋梦柴文祥宋莉王丹丹郭驾宇沈杭燕范美强
Owner CHINA JILIANG UNIV
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