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Preparation of Terbium Ion Coordinated Polymer Fluorescent Nanoprobe and Its K + detection

A technology of fluorescent nanoprobes and ions, which is applied in the direction of fluorescence/phosphorescence, luminescent materials, analytical materials, etc., can solve the problems of complex synthesis process of special polymers, affecting detection efficiency, detection signal interference, etc., and achieves easy mass production, Wide application prospects and the effect of reducing test errors

Active Publication Date: 2021-10-26
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned novel potassium ion fluorescent sensor has been successfully applied to the detection of potassium ion in plasma, aqueous phase, or soil samples, it is not effective for the residual K in special polymers produced on an industrial scale. + The content test has not been reported, mainly because the special polymer synthesis process is complex, and the residual small molecule monomers, intermediate products or reaction solvents in the product will interfere with the detection signal, thereby affecting the detection efficiency

Method used

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  • Preparation of Terbium Ion Coordinated Polymer Fluorescent Nanoprobe and Its K <sup>+</sup> detection
  • Preparation of Terbium Ion Coordinated Polymer Fluorescent Nanoprobe and Its K <sup>+</sup> detection
  • Preparation of Terbium Ion Coordinated Polymer Fluorescent Nanoprobe and Its K <sup>+</sup> detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of preparation method of novel polyarylether nitrile copolymer specifically comprises the following steps:

[0043] Step 1. Add 50 mmoles of potassium 2,5-dihydroxybenzenesulfonate, 47.5 mmoles of difluorodibenzonitrile, 75 mmoles of potassium carbonate, 10 milliliters of toluene and 30 milliliters of N-methyl Pyrrolidone, mixed well;

[0044] Step 2. Stir and reflux the mixed solution obtained in step 1 at 150° C. for 3 hours to obtain mixed solution A;

[0045] Step 3, add 50 millimoles of difluorobenzonitrile, 47.5 millimoles of 4,4-bis(4-hydroxyphenyl) valeric acid, 106.9 millimoles of potassium carbonate, 10 milliliters of toluene, 30 millimoles successively in another reaction flask Milliliter N-methylpyrrolidone, mix well;

[0046] Step 4. Stir and reflux the mixed solution obtained in step 3 at 150° C. for 3 hours to obtain mixed solution B;

[0047] Step 5. After mixing the mixed solution A obtained in step 2 and the mixed solution B obtained in step ...

Embodiment 2

[0051] Tb 3+ The preparation method of coordination polyarylether nitrile nanostructure specifically comprises the following steps:

[0052] Step 1. Add 10 mg of the novel polyarylether nitrile copolymer obtained in Example 1 and 1 mL of N,N-dimethylformamide to a reaction flask in sequence, and fully dissolve it under magnetic stirring to obtain a mixed solution C;

[0053] Step 2, adding 50 μL of NaOH aqueous solution with a concentration of 1 mol / L, 8.86 mL of deionized water and 90 μL of Tb(NO 3 ) 3 ·6H 2 O, obtain mixed solution D;

[0054] Step 3. Under magnetic stirring at a rotational speed of 1500 rpm, add the mixed solution D obtained in step 2 dropwise to the mixed solution C obtained in step 1, and react for 10 minutes to obtain the Tb 3+ Coordination polyarylether nitrile nanostructure;

[0055] Set the emitted light wavelength to 545nm, the slit width to 10nm, the PMT voltage to 700V, the response time to 0.1s, and obtain Tb by wavelength scanning 3+ The ex...

Embodiment 3

[0058] Tb 3+ K of coordination polyarylether nitrile + The preparation method of ratiometric fluorescent probe specifically comprises the following steps:

[0059] Adding 200 μL concentration to the reaction solution obtained in step 3 in Example 2 is a rhodamine B solution of 60 mg / L, centrifuged, and after the product obtained is washed 3 times with deionized water, the lower layer of precipitation is obtained, and 30 milliliters of deionized water is added. can get the Tb 3+ K of coordination polyarylether nitrile + Ratio-type fluorescent probe reaction solution.

[0060] Set the emitted light wavelength to 545nm, the slit width to 10nm, the PMT voltage to 700V, the response time to 0.1s, and obtain Tb by wavelength scanning 3+ K of coordination polyarylether nitrile + The excitation spectrum of the ratiometric fluorescent probe; set the excitation light wavelength to 332nm, the slit width to 10nm, the PMT voltage to 700V, and the response time to 0.1 s, and obtain the...

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Abstract

Preparation of a terbium ion-coordinated poly(arylene ether nitrile) fluorescent nanoprobe and its K + The detection method belongs to the field of metal ion coordination polymers. The present invention uses the block polyarylene ether nitrile copolymer that side chain contains carboxyl group and sulfonic acid group as raw material, through solvent replacement method and Tb 3+ After cross-linking, the rhodamine B dye is adsorbed to obtain fluorescent nanoprobes. With the Tb in the aqueous phase 3+ In the polyarylether nitrile added in the DMF phase, the polyarylether nitrile containing a large number of carboxysulfonic acid groups replaced the water molecules and Tb 3+ coordination, and the presence of a large number of aromatic rings sensitizes Tb 3+ , got Tb 3+ Coordination polyarylene ether nitrile nanoparticles. At the same time, due to the interpenetrating network formed by coordination, the structure has a large specific surface area to facilitate the adsorption of rhodamine B with red emission. Use K + The specific enhancement response to the luminescence intensity of the fluorescent probe was constructed to construct a ratiometric fluorescent nanoprobe, which realized the K + Detection, and detection of residual potassium ions in polyarylether nitrile powder in industrial production.

Description

technical field [0001] The invention belongs to the field of metal ion coordination polymers, in particular to a preparation method of a terbium ion coordination polyarylether nitrile fluorescent nanoprobe and its application in K + application in detection. Background technique [0002] Special engineering plastics have a series of excellent properties such as good heat resistance, high strength, corrosion resistance, good insulation, wear resistance, and radiation resistance, and play an increasingly important role in the fields of electronics, aerospace, and military affairs. Polyarylene ether is a typical type of special engineering plastics. Polyarylether special engineering plastics represented by polyether ether ketone, polyether sulfone, polyarylether nitrile, etc. are all prepared by nucleophilic substitution polycondensation reaction. Due to the polymerization of polyarylether special engineering plastics, excessive K is often used 2 CO 3 As a catalyst, there wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40C08G83/00C09K11/06G01N21/64
CPCC08G65/4031C08G83/008C09K11/06C09K2211/182G01N21/643
Inventor 贾坤谢俊妮刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA