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Europium (iii) metal-organic framework eu-mof probe material and its preparation method and application

A technology of metal-organic frameworks and probes, which is applied in the fields of material analysis, material excitation analysis, and material analysis through optical means, etc. It can solve the problems of limiting the application range of materials, low stability of materials, and strict synthesis conditions, etc., and achieves excellent results. Selectivity and anti-interference ability, easy control of chemical composition, high sensitivity effect

Active Publication Date: 2022-07-19
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently for S 2- The detection of p-aminomethylaniline spectrophotometry is mainly used, the detection limit concentration of this method is 0.02 ~ 0.8mg / L, this method has an obvious shortcoming: if there is SO in the sample 3 2- will affect the measurement results
However, the disadvantages of this kind of metal-organic framework are that it usually takes several days to a week to synthesize the product, the synthesis conditions are relatively strict, the raw materials are expensive, and the stability of the material is not high, especially the water stability severely limits the application range of the material, etc.

Method used

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  • Europium (iii) metal-organic framework eu-mof probe material and its preparation method and application
  • Europium (iii) metal-organic framework eu-mof probe material and its preparation method and application
  • Europium (iii) metal-organic framework eu-mof probe material and its preparation method and application

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preparation example Construction

[0040] The metal-organic framework Eu-MOF material provided by the present invention, its preparation method comprises the following steps:

[0041] 1) The ligand 2,6-benzothiophene dicarboxylic acid H 2 L and Eu (NO 3 ) 3 ·6H 2 O is added in the reactor, mixed;

[0042] When implemented, H 2 L and Eu (NO 3 ) 3 ·6H 2 The molar ratio of O can be any ratio within 1:1 to 1.5:1;

[0043] The reaction kettle provided by the invention is a high pressure reaction kettle or a glass reaction bottle;

[0044] 2) continue to add N,N-dimethylformamide DMF and H in the reactor 2 Mixed solution of O, mixed and sealed;

[0045] When implemented, DMF and H 2 The molar ratio of O can be any ratio from 1:1 to 1:2; DMF to H 2 The mass ratio of L is any ratio within 100:1 to 120:1;

[0046] 3) The sealed reactor in step 2) was placed in a blast drying oven, and with a heating rate of 0.5°C / min, a constant temperature reaction was performed for 4 hours when the temperature was raised ...

Embodiment 1

[0049] 1) The mass of 0.0222g ligand 2,6-benzothiophene dicarboxylic acid H 2 L and Eu(NO) with a mass of 0.0446 g 3 ) 3 ·6H 2 0 is put into the autoclave with a volume of 25mL, respectively, and mixes;

[0050] In this embodiment, the high-pressure reaction kettle is lined with polytetrafluoroethylene, and the outer material is stainless steel; 2,6-benzothiophene dicarboxylic acid and Eu(NO) 3 ) 3 ·6H 2 The molar ratio of O is 0.1mmol:0.1mmol=1:1;

[0051] 2) continue to add the N,N-dimethylformamide DMF of 2.5mL and the H of 2.5mL in the autoclave 2 Mixed solution composed of O, mixed and sealed; DMF and H 2 O volume ratio is 1:1; DMF and H 2 The mass ratio of L is 100:1;

[0052] 3) Place the sealed autoclave in step 2) in a blast drying oven, and at a heating rate of 0.5°C / min, the temperature of the drying oven is raised from 20°C to 80°C within 2 hours, and the reaction is performed at a constant temperature for 4 hours. hour; then the cooling rate of 1°C / min r...

Embodiment 2

[0054] The difference between this example and Example 1 is that the cooling time in step 3) is 10h, that is, a cooling rate of 0.1°C / min is used to reduce the temperature of the drying oven from 80°C to 20°C. The crystals were weighed and the Eu-MOF probe material yield was calculated to be 50%.

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Abstract

The invention belongs to the technical field of fluorescent probe materials, and relates to a europium (III) metal-organic framework Eu-MOF probe material and a preparation method and application thereof. The general chemical formula of the Eu-MOF probe material is [Eu 2 (L) 3 ·DMF·2H 2 O] n ·2DMF·4H 2 O, the crystal structure is the orthorhombic Pnma space group, α=β=γ=90°, Z=4. The probe material provided by the present invention is suitable for Fe 3+ and S 2‑ The detection has excellent selectivity, anti-interference ability, high sensitivity and potential application value, and the preparation process is simple, the process conditions are controllable, the synthesis time is short, and large-scale production is possible.

Description

technical field [0001] The invention belongs to the technical field of fluorescent probe materials, and relates to a europium (III) metal-organic framework Eu-MOF probe material and a preparation method and application thereof. Background technique [0002] Iron is an essential trace element in the human body, and both deficiency and excess of iron can cause various diseases. The detection of iron content has become a hot spot of people's attention. However, traditional iron content detection and analysis methods, including liquid chromatography, inductively coupled plasma-atomic mass spectrometry (ICP-MS), and atomic absorption spectrometry (AAS), have the disadvantages of complicated operation and long detection process. , low selectivity, easy to be interfered by other ions and high cost of detection, which limits its widespread use. Therefore, it is urgent to develop a detection method that is easy to use, low cost, high selectivity and sensitivity. [0003] Sulfur is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00G01N21/64
CPCC08G83/008G01N21/643G01N2021/6432
Inventor 李磊磊刘双王文珍苏红丹
Owner XI'AN PETROLEUM UNIVERSITY
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