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Pillar 5 arene polymer, synthesis and application thereof in fluorescence detection and mercury ion removal

A technology of high polymers and aromatics, applied in the direction of fluorescence/phosphorescence, luminescent materials, chemical instruments and methods, etc., can solve problems such as inability to separate mercury ions

Active Publication Date: 2017-09-29
山东奥达复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, many fluorescent probes only have the ability to identify and detect mercury ions, and cannot separate mercury ions in solution. Therefore, it is very necessary to have a fluorescent probe that can detect mercury ions and remove mercury ions.

Method used

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  • Pillar 5 arene polymer, synthesis and application thereof in fluorescence detection and mercury ion removal
  • Pillar 5 arene polymer, synthesis and application thereof in fluorescence detection and mercury ion removal
  • Pillar 5 arene polymer, synthesis and application thereof in fluorescence detection and mercury ion removal

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1, the synthesis of pillar 5 aromatic hydrocarbon high polymer

[0038] (1) Synthesis of Copolymerized Pillar 5 Aromatics

[0039] Synthesis of Intermediate 1: Hydroquinone (2.2 g, 20.0 mmol), K 2 CO 3 (13.8 g, 100 mmol), KI (0.83 g, 5 mmol), PEG-400 (4 mL, 10 mmol), 1,4-dibromobutane (17.28 g, 80 mmol) and acetone (300~400 mL) were added to a 500 mL round bottom In the flask, stirred and reacted at 60°C for 36 h, cooled to room temperature, removed the inorganic salt by suction filtration, evaporated the solvent under reduced pressure, and separated by column chromatography to obtain a white solid which is intermediate compound 1 with a yield of 80%. m.p: 83~85 ° C; 1 H NMR (400MHz, CDCl 3 ) δ (ppm): δ 6.81 (s, 4H), 3.94 (dd, J = 10.0, 5.8 Hz, 4H), 3.48(t, J = 6.6 Hz, 2H), 3.26 (t, J = 6.8 Hz, 2H), 2.09-1.85 (m, 8H).

[0040] Synthesis of Copolymer 5 Aromatics 2: Add 1,2-dichloroethane (300 mL) into a 500 mL round low flask, add intermediate c...

Embodiment 2

[0049] Embodiment 2, identify Hg with PP5 2+

[0050] Dimethyl sulfoxide turbid solution in PP5 (water content 50%, PP5 concentration 4×10 -4 mol L -1 ), adding Mg 2+ , Ca 2+ , Zn 2+ , Co 2+ , Fe 3+ , Pb 2+ , Cd 2+ , Hg 2+ , Ni 2+ , Tb 3+ , Cu 2+ , Eu 3+ , Fe 2+ , Cr 3+ , Ag + , La 3+ DMSO solution (0.004 mol L -1 ), if the fluorescence of PP5 turbid solution is quenched, it means that Hg was added 2+ , if the fluorescence of the PP5 turbid solution does not change, it means that the addition of Hg is not 2+ .

Embodiment 3

[0051] Embodiment 3, remove the Hg in the aqueous solution with PP5 2+

[0052] Add 5 mg of PP5 polymer to 5 mL of Hg 2+ aqueous solution (1 x 10 -4 mol L −1 ), stirred at room temperature for 5 hours, filtered to remove insoluble matter, and detected the clear aqueous solution by ICP method, and found that Hg 2+ is almost eliminated (for Hg 2+ The removal rate is 96.25%).

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Abstract

The invention discloses a pillar 5 arene polymer with fluorescence detection and mercury ion removal functions. The pillar 5 arene polymer is obtained through steps of carrying out reflux reaction on copolymerized pillar 5 arene and ethyl thioglycolate as raw materials to obtain functionalized pillar 5 arene carrying out reflux reaction on the functionalized pillar 5 arene and hydrazine hydrate as the raw materials to obtain pillar 5 arene; enabling the pillar 5 arene to react with terephthalaldehyde to obtain a yellow-green sediment; and filtering, washing and drying to obtain the pillar 5 arene polymer. According to the polymer, a good fluorescent signal base is provided for a benzene ring group of the pillar 5 arene, yellow-green fluorescent light of the polymer is quenched through complexing a sulphur atom and a mercury ion, and fluorescent recognition of the mercury ion is achieved. The polymer has the characteristic of being difficult to dissolve into a water solution and an organic solution, and the mercury ion can be separated from a water phase, thereby achieving the purpose of removing the mercury ion.

Description

technical field [0001] The present invention relates to a high polymer with fluorescence recognition and removal of mercury ions, in particular to a 5-aromatic polymer with fluorescence recognition and removal of mercury ions and a synthesis method thereof. The present invention also relates to the 5-aromatic high polymer The invention relates to the application of polymers in fluorescent recognition of mercury ions and removal of mercury ions in aqueous solution, and belongs to the technical field of polymer materials and cation detection and separation. Background technique [0002] Among the many transition metal ions, mercury ions are very harmful to the human body and the natural environment, so its identification, detection and separation have always been a hot topic for environmental researchers. Among various methods for detecting mercury ions, the fluorescent probe method has the characteristics of high sensitivity and easy operation, and has attracted more and more...

Claims

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Application Information

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IPC IPC(8): C08G12/26C09K11/06G01N21/64
Inventor 魏太保陈进发韩冰冰张有明林奇姚虹
Owner 山东奥达复合材料有限公司
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