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A kind of eu/tb-tcp-cooh complex luminescent material and its preparation method and application

A technology of luminescent materials and complexes, which is applied in the direction of material analysis by optical means, compounds of group 5/15 elements of the periodic table, and analytical materials. and other problems, to achieve the effect of easy promotion and use, good reproducibility and stability, and fast detection method

Active Publication Date: 2020-07-28
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the deficiencies of the above-mentioned prior art, the present invention provides a ligand of rare earth europium / terbium, which solves the problem that the existing ligands can be matched with terbium ions and europium ions at the same time. Body provides more choices
[0007] The present invention also provides a Eu / Tb-TCP-COOH complex luminescent material and its preparation method and application, which solve the problems of high cost, long reaction time and lack of wide applicability of existing VOC detection methods

Method used

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  • A kind of eu/tb-tcp-cooh complex luminescent material and its preparation method and application
  • A kind of eu/tb-tcp-cooh complex luminescent material and its preparation method and application
  • A kind of eu/tb-tcp-cooh complex luminescent material and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0044] 1) Preparation of ligand TCP-COOH: Add 9.038g (42mmol) dimethyl 5-hydroxyisophthalate and 6.3g (45mmol) potassium carbonate into 120mL of anhydrous tetrahydrofuran, stir well to dissolve the solid, and then raise the temperature to 70°C, and added 2.43g (7mmol) hexachlorocyclotrimeric phosphazene, condensed and refluxed for 48h, filtered after the reaction was complete, the filtrate was distilled to remove the solvent, and then heated in a vacuum oven at 60°C to obtain a white solid. Add the white solid to 30mL of THF solution, add 2.3g NaOH to 20ml of distilled water and add dropwise to the above THF solution, after the reaction, remove THF with a rotary evaporator, and pour the remaining solution into deionized water (150mL) , acidified with dilute hydrochloric acid to a pH of about 1, and after stirring, a precipitate was obtained and collected, washed three times with deionized water, and dried overnight in a vacuum oven at 60°C to obtain hexanuclear trimeric phospha...

Embodiment 2

[0055] 1) Preparation of ligand TCP-COOH: add 6.4g dimethyl 5-hydroxyisophthalate and 5g potassium carbonate into 150mL tetrahydrofuran, stir well to dissolve the solid, then heat up to 70°C, and add 1.71g Chlorocyclotrimeric phosphazene, condensed and refluxed for 64h, filtered after the reaction was complete, the filtrate was distilled to remove the solvent, and then heated in a vacuum oven at 60°C to obtain a white solid, which was added to 30mL of THF solution and dissolved in 20ml of Add 2.3g NaOH in distilled water and add it dropwise to the above THF solution. After the reaction, remove THF with a rotary evaporator, pour the remaining solution into deionized water (150mL), acidify with dilute hydrochloric acid to a pH of about 1, and stir A precipitate was obtained and collected, washed three times with deionized water, and dried overnight in a vacuum oven at 60° C. to obtain hexanuclear trimeric phosphazene TCP-COOH.

[0056] 2) Preparation of hexanuclear trimeric phos...

Embodiment 3

[0059] 1) Preparation of the ligand TCP-COOH: Add 6.4g of dimethyl 5-hydroxyisophthalate and 6g of potassium carbonate into 120mL of anhydrous tetrahydrofuran, stir well to dissolve the solid, then raise the temperature to 70°C, and add 1.5 g hexachlorocyclotrimeric phosphazene, condensed and refluxed for 52h, filtered after the reaction was complete, the filtrate was distilled to remove the solvent, and then heated in a vacuum oven at 60°C to obtain a white solid, which was added to 30mL of THF solution, in Add 2.3g NaOH to 20ml of distilled water and add dropwise to the above THF solution. After the reaction, remove THF with a rotary evaporator, pour the remaining solution into deionized water (150mL), and acidify with dilute hydrochloric acid until the pH is about 2 After stirring, a precipitate was obtained and collected, washed three times with deionized water, and dried overnight in a vacuum oven at 60°C to obtain hexanuclear trimeric phosphazene TCP-COOH.

[0060] 2) Pr...

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Abstract

The invention discloses an Eu / Tb-TCP-COOH complex luminescent material as well as a preparation method and application thereof. Phosphonitrilic chloride trimer, dimethyl 5-hydroxyisophthalate and potassium carbonate are used as raw materials for synthesizing an aromatic carboxylic acid derivative ligand TCP-COOH; then, the aromatic carboxylic acid derivative ligand TCP-COOH, EuCl3.6H2O and TbCl3.6H2O react to obtain a complex Eu / Tb-TCP-COOH; then, the ligand and a graphene water solution are blended for spinning; an Eu / Tb hollow graphene fluorescence fiber with certain intensity is obtained. The prepared complex and the hollow graphene fluorescence fiber have high selective recognition capability on VOC gas; particularly, a cancerogen of styrene can be fast responded; the sensitivity is high; the recovery speed is high; the repeated use can be realized; the cost of the preparation method is relatively low; the operability is high; the risk is low; the popularization and the use are easy, so that great potential is shown in indoor environment detection and biomedicine fields.

Description

technical field [0001] The invention relates to the technical field of rare earth luminescent materials, in particular to a rare earth europium / terbium complex of a luminescent material and a preparation method and application thereof. Background technique [0002] Rare earth elements are a general term for 17 special elements. Due to the unique structure of rare earth ions due to their 4f electron layer, they have unique luminescent properties. Rare earth ions have abundant electronic transition energy levels, and different electronic energy level transitions present various Absorption and emission spectra. These unique luminescent properties make rare earth compounds widely used in medical treatment, biological imaging, optical fiber, lighting devices and so on. Rare earth complexes are obtained by coordination and bonding of ligands and rare earth ions. The principle of luminescence is that the ligand absorbs energy in the ultraviolet region, and then the ligand transfer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/659C08G83/00G01N21/64
CPCC07F9/65815C08G83/008C09K2211/182G01N21/643G01N2021/6432
Inventor 杨朝龙贾鹏李又兵张丹苏艳高伟宸王中豪张永锋刘欣杨巧梅白竹煜
Owner CHONGQING UNIV OF TECH
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