Rare earth organic framework material having sensing function to acetone, preparation method and application thereof

A technology of rare earth organic and framework materials, which is applied in the preparation of test samples, luminescent materials, and material excitation analysis. It can solve problems such as low stability, hindering practical applications, and structural collapse. And the effect of low cost and strong water resistance

Inactive Publication Date: 2013-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the stability of existing metal-organic framework materials is generally not high, especially in the presence of water vapor, which is prone to structural collapse, which greatly hinders its practical application (Y.Li et al., Langmuir, 2007, 23, 12937)

Method used

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  • Rare earth organic framework material having sensing function to acetone, preparation method and application thereof
  • Rare earth organic framework material having sensing function to acetone, preparation method and application thereof
  • Rare earth organic framework material having sensing function to acetone, preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] a: Synthetic compound of the present invention by hydrothermal synthesis method:

[0034] (1) Weigh 0.5mmol Eu 2 o 3 , heated and dissolved with concentrated nitric acid, volatilized and cooled to form europium nitrate;

[0035] (2) weigh 1mmol 5-methyl-pyrazine-2-carboxylic acid, and dissolve it in 15ml double-distilled water together with the above-mentioned Eu salt;

[0036] (3) Add 0.12ml concentrated nitric acid, transfer to 23ml hydrothermal reaction kettle after fully stirring;

[0037] (4) React at a constant temperature of 150° C. for 24 hours. Then, at 10℃·h -1 Cool down to room temperature;

[0038] (5) Open the hydrothermal reaction kettle to obtain a light yellow block crystal, which is the compound of the present invention.

[0039] b: Structure determination of the complex

[0040] The crystal structure was obtained by Bruker SMART 1000 X-ray diffractometer, using Mo Kα rays obtained through graphite monochromatization As the incident radiation, ...

Embodiment 2

[0052] a: Compound synthesis

[0053] (1) Weigh 0.1mmol Eu 2 o 3 , heated and dissolved with concentrated nitric acid, volatilized and cooled to form europium nitrate;

[0054] (2) Weigh 0.2mmol 5-methyl-pyrazine-2-carboxylic acid, and dissolve it in 5ml twice-distilled water together with the above-mentioned Eu salt;

[0055] (3) Add 0.04ml concentrated nitric acid, transfer to 23ml hydrothermal reaction kettle after fully stirring;

[0056] (4) Constant temperature reaction at 120°C for 50h. Then, at 5℃·h -1 Cool down to room temperature;

[0057] (5) Open the hydrothermal reaction kettle to obtain a light yellow block crystal, which is the compound of the present invention.

[0058] b: the structure of the compound

[0059] Through single crystal diffraction characterization, it is found that the crystal belongs to the triclinic system, the space group is P-1, and the unit cell parameters are: α=68.873(3)°, β=81.013(2)°, γ=76.721(3)°. It shows that the compound pr...

Embodiment 3

[0061] a: Compound synthesis

[0062] (1) Weigh 0.5mmol Eu 2 o 3 , heated and dissolved with concentrated nitric acid, volatilized and cooled to Eu salt;

[0063] (2) weigh 1mmol 5-methyl-pyrazine-2-carboxylic acid, and dissolve it in 10ml double-distilled water together with the above-mentioned Eu salt;

[0064] (3) Add 0.08ml concentrated nitric acid, transfer to 23ml hydrothermal reaction kettle after fully stirring;

[0065] (4) React at a constant temperature of 150° C. for 24 hours. Then, at 10℃·h -1 Cool down to room temperature;

[0066] (5) Open the hydrothermal reaction kettle to obtain a light yellow block crystal, which is the compound of the present invention.

[0067] b: the structure of the compound

[0068] Through single crystal diffraction characterization, it is found that the crystal belongs to the triclinic system, the space group is P-1, and the unit cell parameters are: α=68.871(4)°, β=81.012(3)°, γ=76.722(2)°. It shows that the compound prepar...

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PUM

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Abstract

The invention discloses a rare earth organic framework material having sensing function to acetone, a preparation method and application thereof. The material has the following chemical formula: [Eu(pyca)(ox)0.5(H2O)].4(H2O), wherein, pyca is 2,5-pyrazine diacid ligand, and ox is oxalate ligand. The invention selects 5-methyl-pyrazine-2-carboxylic acid and Eu metal to synthesize a three-dimensional metal organic framework with one-dimensional pore canals. When acetone molecules are added in the N-N'-dimethyl formamide solution of Eu metal containing organic framework, the position of the fluorescence-emission peak is not changed, the strength of the emission peak recedes obviously along with the enhancement of the concentration of the acetone molecule, thus the framework material can be used as a fluorescence probe of acetone molecule to detect trace acetone molecules in the solution. The material has stable structure and strong water-resistance. The invention has convenient, fast andsensitive characteristics in chemical detection.

Description

technical field [0001] The invention relates to a rare earth metal organic framework material, in particular to a rare earth organic framework material with sensing function to acetone and stable water resistance and a preparation method thereof, which can be used as Eu 3+ Metal-type acetone molecular fluorescent probe. Background technique [0002] The detection of volatile organic compounds is a very important issue in environmental monitoring and even people's daily life, which has attracted great attention from governments and experts in various countries. Acetone is a volatile organic solvent widely used in industry and laboratories. Acetone can enter the human body through the respiratory tract, digestive tract, and skin, seriously endangering human health. In view of the great harm of acetone to the human body, we often have to analyze and measure its content in environmental monitoring work such as pollution accidents, environmental impact assessment and facility ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06G01N21/64G01N1/28
Inventor 李映伟马德运
Owner SOUTH CHINA UNIV OF TECH
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