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Preparation method and application of Eu<3+>-MOF material

A 3·6H2O, reaction technology, applied in the field of fluorescence sensing, can solve the problems of complex coordination environment and high coordination number of MOF, and achieve high sensitivity, low detection limit and good application prospects

Inactive Publication Date: 2020-03-31
YANTAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(L.E.Kreno, K.Leong, O.K.Farha, M.Allendorf*, R.P.Van Duyne, J.T.Hupp*, Metal-Organic Framework Materials as Chemical Sensors, Chem.Rev.112(2012)1105-1125.) But in practical application Among them, due to the high coordination number and complex coordination environment of MOFs, the rational design and construction of Ln-MOFs are still under development.

Method used

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  • Preparation method and application of Eu&lt;3+&gt;-MOF material
  • Preparation method and application of Eu&lt;3+&gt;-MOF material
  • Preparation method and application of Eu&lt;3+&gt;-MOF material

Examples

Experimental program
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Embodiment 1

[0031] Example 1: Preparation of iron-based metal organic frameworks.

[0032] This embodiment provides a kind of iron-based MOF material, and its chemical composition is: Fe III (OH)[C 6 h 2 (CO 2 ) 2 (CO 2 h) 2 ]·xH 2 O, its concrete preparation process is as follows:

[0033] Chemically pure or analytically pure FeCl 2 4H 2 O and H 4 BTEC as raw material, according to FeCl 2 4H 2 O: H 4 btec: H 2 O=1:0.5:100 (5mL) (5mL refers to the amount of other substances determined by the amount of 5mL of water, which requires conversion) and weighed in a molar ratio, placed in a polytetrafluoroethylene-lined stainless steel reactor, Stir at room temperature until uniform, seal and place in an oven at 200°C for 48 hours of reaction. After natural cooling, a reddish-brown product is obtained. The obtained product was centrifuged and washed several times with acetone and vacuum-dried at room temperature to obtain an iron-based metal-organic framework.

[0034] The obtaine...

Embodiment 2

[0035] Example 2: Eu 3+ - Preparation of MOF materials.

[0036] This example provides a post-utilization preparation method for obtaining Eu 3+ -MOF material, its specific preparation process is as follows:

[0037] By mixing 0.1g Fe-based MOF material and 0.0892g Eu(NO 3 ) 3 ·6H 2 A mixture of O was stirred in 10 mL of aqueous solution for 24 hours to prepare Eu 3+ -MOF materials. The resulting brown solid was then separated from the mixed dispersion by centrifugation and washed with an aqueous solution to remove excess Eu 3+ , and the obtained brown powder was vacuum-dried at 60 °C for 8 h.

[0038] For the obtained Eu 3+ -MOF materials were characterized by powder X-ray (PXRD) pattern and thermogravimetric (TG) analysis. figure 1 The PXRD pattern of the obtained sample is given, compared with the crystal structure pattern of the iron-based MOF material, and the synthesized Eu 3+ -MOF materials did not change in crystal structure, indicating that Eu 3+ Doping doe...

Embodiment 3

[0039] Embodiment 3: Fluorescence sensing experiment.

[0040] This embodiment uses the Eu prepared in Example 2 3+ -MOF material for fluorescence sensing experiments, the specific experimental process is as follows:

[0041] The powder prepared by 3mg embodiment 2 was dispersed in M(NO 3 ) x Aqueous solution (3ml, 1×10 -2 mol / L) (M n+ =Ag + , Pb 2+ , Ca 2+ , Zn 2+ , Hg 2+ , Ni 2+ , Mg 2+ ,Co 2+ , Cd 2+ , Na + , Cr 3+ , Al 3+ , Fe 3+ ). The mixture was then sonicated for 10 min to form a suspension doped with metal ions for luminescence measurements. All luminescence data were recorded at room temperature.

[0042] The samples obtained in Example 2 were tested for the emission spectrum. Luminescence spectra of mixed suspensions doped with metal ions were recorded at room temperature. Figure 4 As shown, the visible material exhibits Eu 3+ strong characteristic emission peaks. Figure 5 The photoluminescence spectra of mixed suspensions of various metal i...

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Abstract

The invention relates to a preparation method and application of an Eu<3+>-MOF material. The preparation method comprises the following steps: preparing an iron-based MOF material from ferrous chloride and pyromellitic acid and then preparing the Eu<3+>-MOF material from the prepared iron-based MOF material and europium nitrate. The prepared Eu<3+>-MOF material shows strong characteristic emissionlight of Eu<3+> and has good water stability and thermal stability. Ag<+> has good concentration dependence on the enhancement efficiency of Eu<3+>-MOF fluorescence. The detection range of Ag<+> is 0-150 [mu]M, the detection limit is 0.09 [mu]M, and the response speed of the material to Ag<+> is very fast (3 min).

Description

technical field [0001] A kind of Eu of the present invention 3+ -The preparation method of MOF material, and relates to the prepared material as Ag + applications of fluorescent sensing materials. The invention belongs to the technical field of fluorescence sensing. Background technique [0002] With the rapid development of industry, heavy metal ions are more and more harmful to the environment and human health. Therefore, the detection of heavy metal ions plays an important role in life science, biomedicine and environmental science. (Duruibe, Ogwuegbu, Egwurugwu, Heavy metal pollution and human biotoxic effects, Int. J. Phys. Sci. 2 (2007) 112-118.) Silver (Ⅰ) is an important one of the ions. Silver ions can accumulate in organisms through the food chain and drinking water, causing silver ion poisoning, resulting in cell damage and organ failure. (J.Wu, G.Q.Chen, F.Z.Cui, T.N.Kim, J.O.Kim, A mechanistic study of the antibacterial effect of silver ions on Escherichia...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/182G01N21/64G01N21/6428G01N21/643G01N2021/6417
Inventor 徐志军葛凯明闫萌军李大磊贺笑春初瑞清
Owner YANTAI UNIV
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