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Oxygen concentration responsive polymer photoluminescence coating as well as preparation and application thereof

A technology of photoluminescence and oxygen concentration, which is applied in the direction of luminescent coatings, coatings, luminescent materials, etc., to achieve the effects of avoiding fluorescence quenching, aerobic concentration response, and increasing capacity

Active Publication Date: 2019-01-18
UNIVERSITY OF CHINESE ACADEMY OF SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Metal ruthenium complexes have strong photoluminescence, large Stokes shift and high oxygen sensitivity, and are often used in the research of oxygen sensing, and most of them are used in the detection of oxygen-deficient parts in organisms, such as Due to the strong metabolism of the tumor in the organism, the oxygen concentration decreases, and the oxygen-sensitive probe that reaches the tumor will generate strong fluorescence due to low oxygen under a certain excitation light, so as to achieve the purpose of tumor detection; the oxygen-sensitive material in the optical sensor There are also reports on the application in the coating, and there are few reports on the coating, and most of the oxygen molecular probes are physically dispersed in the matrix. There is no report on the oxygen-sensitive probe molecules bonded to the matrix resin to prepare the oxygen-sensitive coating.

Method used

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  • Oxygen concentration responsive polymer photoluminescence coating as well as preparation and application thereof
  • Oxygen concentration responsive polymer photoluminescence coating as well as preparation and application thereof
  • Oxygen concentration responsive polymer photoluminescence coating as well as preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0051]Weigh 30g of epoxy resin and preheat at 50°C for 20min, take 20% of the mass of epoxy resin as nano-silica powder, add 8.75g of curing agent DDM and mechanically stir evenly, add to the preheated epoxy resin and stir vigorously for 7h, then put in vacuum Vacuum in the oven to remove air bubbles, then spray on the glass substrate and cure at room temperature for 30 minutes. The coating thickness is about 20 μm.

[0052] [Ru(dcbpy)(bpy) 2 ] 2+ ]Cl 2 Dissolve in methanol to prepare a solution with a concentration of 1.0mg / ml, brush on the surface of epoxy resin, and cure at 50°C for 8 hours in the dark.

[0053] Coating oxygen permeable protective layer: Add 17ml ether to 3gRTV glue, stir evenly, take 20mg mixture and brush on an area of ​​about 6cm 2 The surface of the coating should be cured at room temperature in the dark for 0.5-3 hours. The average thickness of the prepared oxygen concentration sensitive coating is about 29 μm.

[0054] In this embodiment, accord...

Embodiment 2

[0059] Weigh 30g of epoxy resin and preheat at 50°C for 10-30min, take 19% of the mass of epoxy resin, add 8.75g of curing agent DDM and mechanically stir it evenly, add it into the preheated epoxy resin and stir vigorously for 7h, put in Vacuum in a vacuum oven to remove air bubbles, then spray on a stainless steel substrate, and cure at room temperature for 30 minutes. The coating thickness was 19 μm.

[0060] [Ru(dcbpy) 2 (bpy)] 2+ ]Cl 2 Synthesis:

[0061] Preparation of (4,4'-dicarboxy-bipyridine) ruthenium complex Ru(dcbpy) 2 Cl 2 : Ruthenium trichloride trihydrate reacts with 4,4'-dicarboxy-bipyridine small molecules, and the molar ratio of feeding is n(RuCl3 3H2O):n(dcbpy)=1:2~1:3, and the reaction solvent is N,N-Dimethylformamide, the reaction temperature is 100-120°C, under a nitrogen atmosphere, the reaction is stirred for 24 hours, the reaction is stopped, the insoluble matter is filtered off, the solvent is drained, and acetone is recrystallized.

[0062] P...

Embodiment 3

[0069] Weigh 30g of epoxy resin and preheat at 50°C for 20 minutes, take 21% of the mass of epoxy resin, add 8.75g of curing agent DDM and mechanically stir it evenly, add it to the preheated epoxy resin and stir vigorously for 7 hours, then put it in a vacuum oven Vacuum out the air bubbles, then spray on the alumina substrate, and cure at room temperature for 30 minutes.

[0070] Preparation of tri(4,4'-dicarboxy-bipyridine) ruthenium complex [Ru(dcbpy) dichloride 3 ]Cl 2 : Ruthenium trichloride trihydrate reacts with small molecules of 4,4'-dicarboxy-bipyridine, the molar ratio of the feed is n(RuCl3 3H2O):n(dcbpy)=1:3, and the reaction solvent is N,N- In dimethylformamide, the reaction temperature is 100-120° C., under a nitrogen atmosphere, the reaction is stirred for 24 hours, the reaction is stopped, the insoluble matter is filtered off, the solvent is drained, and acetone is recrystallized.

[0071] [Ru(dcbpy) 3 ]Cl 2 The complex was dissolved in methanol to prepar...

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Abstract

The invention provides an oxygen concentration responsive polymer photoluminescence coating. The coating consists of an oxygen concentration sensitive function layer and a matrix resin layer mixed with nanoparticles, wherein the oxygen concentration sensitive function layer is distributed on the surface of the matrix resin layer mixed with nanoparticles. The oxygen concentration sensitive functionlayer is prepared from a metal ruthenium complex (oxygen sensitive probe molecules). The oxygen sensitive probe molecules are distributed on the surface of the polymer resin coating in the form of chemical bond and / or physical interaction, and the surface has a coarse structure of micro-nano scale due to doping of nanoparticles. The coarse surface structure and the surface distribution form of the probe improve the dynamic contact efficiency of the probe and oxygen molecules, so that the change speed of fluorescence emission light intensity is increased when the probe molecules respond to thechange of oxygen concentration on the surface of the coating, and noncontact detection of change of oxygen concentration or air pressure on the surface of the coating is realized through change of fluorescence intensity or fluorescence life of the coating. The coating is simple to prepare, has reversible response to oxygen and can be reused for a long time.

Description

technical field [0001] The invention relates to the field of coating preparation, in particular to an oxygen concentration-responsive polymer photoluminescent coating and its preparation and application. Background technique [0002] Sensitive detection of oxygen concentration (oxygen partial pressure) is of great significance in research fields such as analytical chemistry, biomedicine, and environmental monitoring. Its detection technology is also constantly improving and developing, from chemical methods and electrochemical sensors to current photochemical sensors. Photochemical oxygen molecular sensors have good responsivity and high sensitivity, which has aroused widespread research interest, and its application is also deepening. The core of this type of detection technology is fluorescent or phosphorescent molecules that rely on fluorescence properties that are highly sensitive to oxygen concentration. . It is common to use complexes composed of transition metals Ru(...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D163/00C09D5/22C09D7/63C07F15/00C09K11/06G01N21/64G01L11/02
CPCC07F15/0053C08K3/22C08K3/36C08K2003/2241C08K2201/011C09D163/00C09K11/06C09K2211/185G01L11/02G01N21/6428C08L1/02
Inventor 杨迪屈小中赵嫣然
Owner UNIVERSITY OF CHINESE ACADEMY OF SCIENCES
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