A kind of preparation method and application of two-dimensional porous cd-mofs

An application method and reaction technology, applied in the field of environmental analysis, can solve the problems of low adsorption efficiency and achieve the effects of large adsorption capacity, high adsorption performance and good application prospects

Active Publication Date: 2022-05-20
NANCHANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, although there have been some breakthroughs in the research and application of MOFs and covalent organic frameworks (COFs) materials, the adsorption efficiency of most materials is relatively low (H.Y.Sun, Y.Liu, J.Lin, Z.H.Yue, W.A.Li, J.C. Jin, Q.Sun, Y.J.Ai, M.L.Feng, X.Y.Huang, Highly selective recovery of lanthanides by using a layered vanadate with acid and radiation resistance, Angew.Chem.Int.Ed.2020,59,1878-1883)

Method used

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  • A kind of preparation method and application of two-dimensional porous cd-mofs
  • A kind of preparation method and application of two-dimensional porous cd-mofs
  • A kind of preparation method and application of two-dimensional porous cd-mofs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: the preparation method of two-dimensional porous Cd-MOFs material

[0034] Add 3.2g of pyromellitic anhydride (PMDA) and 5.32g of 5-aminoisophthalic acid into 30mL of glacial acetic acid solution respectively, mix the two and stir and heat the mixed solution at 120°C for 24h, and the obtained white precipitate distilled water and CHCl 3 Wash three times, and then dry in an oven at 80°C to obtain a light yellow solid powder, and make imide ligand H 4 BDCPPI; 0.025 mmol of H 4 BDCPPI, 0.07mmol of Cd(NO 3 ) 2 4H 2 The mixed solution of 0 and 3mL of DMF was placed in a 25mL reaction kettle, the temperature was programmed to rise to 115°C within 6h, and the constant temperature reaction was carried out at 115°C for 36h, and the temperature was programmed to cool down to room temperature within 72h, and the obtained light yellow solid was vacuum filtered, and then used DMF and water were washed and dried to make Cd-MOFs crystal material.

[0035] Using X-ray...

Embodiment 2

[0036] Example 2: Cd-MOFs to rare earth Tb 3+ Ratiometric Fluorescence Detection Applications

[0037] (1) Preparation and characterization of Cd-MOF fluorescent probe

[0038] Ultrasonic dispersion of 10 mg of Cd-MOFs material in 10 mL of ultrapure water was made into a 1 mg / mL suspension, and 200 μL of the Cd-MOFs suspension was diluted to 3 mL with ultrapure water to prepare a Cd-MOF fluorescent probe solution. Fluorescence spectroscopy of Cd-MOFs fluorescent probes and Tb 3+ The fluorescence characteristics before and after the reaction were characterized, and the results were as follows: figure 2 shown. Under the excitation wavelength of 264nm, the Cd-MOFs fluorescent probe has a strong fluorescent signal at 405nm (curve a); when adding Tb to the Cd-MOFs fluorescent probe 3+ After solution, the solution exhibits dual emission fluorescence signals, that is, simultaneously emitting Cd-MOFs and Tb 3+ Fluorescence signal of Cd-MOFs, where the intensity of the emission ...

Embodiment 3

[0045] Example 3: Enrichment application of Cd-MOFs to rare earth elements

[0046] (1) Cd-MOFs rare earth Tb 3+ The adsorption capacity measurement of

[0047] Under neutral conditions, 50 mg of Cd-MOFs was added to 50 mL containing different concentrations (0-800 ppm) of Tb 3+ In the solution, the suspension was stirred for 3h and filtered through a 0.22μm microporous membrane; the rare earth Tb in the filtrate was measured by inductively coupled plasma mass spectrometry 3+ Concentration, calculated Cd-MOFs to rare earth Tb 3+ of adsorption capacity. Cd-MOFs vs. Tb 3+ The adsorption capacity increases with Tb 3+ The concentration increases until the adsorption equilibrium state is reached ( Figure 5 A), and Qe / Ce and Ce have a good linear correlation ( Figure 5 B), Cd-MOFs on Tb 3+ The maximum adsorption capacity is 303mg / g.

[0048] (2) The enrichment rate of all rare earths by Cd-MOFs

[0049] In the presence of different rare earth ions, Cd-MOFs can also adsor...

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Abstract

The invention discloses a preparation method and application of two-dimensional porous Cd-MOFs, belonging to the technical field of environmental analysis. The two-dimensional porous Cd-MOFs material prepared based on imide ligands and metal-centered cadmium ions not only has its own fluorescence emission characteristics, but also can sensitize rare earth Tb through the "antenna effect". 3+ glow. When adding Tb to Cd‑MOFs 3+ When, Tb 3+ The fluorescence of Cd-MOFs is significantly enhanced, while the fluorescence intensity of Cd-MOFs is weakened. Accordingly, the analytical Tb 3+ The ratiometric fluorescence method of the content achieves the Tb 3+ sensitive detection. In addition, due to the presence of a large number of amino groups on the periphery of Cd-MOFs, it is very easy to combine rare earth elements, and the porous structure of Cd-MOFs also makes it have high adsorption performance and large adsorption capacity for rare earth elements, so as to achieve high-efficiency enrichment of low-concentration rare earth elements. Effect. The above results show that the two-dimensional porous Cd-MOFs framework material synthesized by the method of the present invention has 3+ It has good application potential in detection and enrichment and separation of rare earth elements.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis, and in particular relates to a preparation method and application of two-dimensional porous Cd-MOFs. Background technique [0002] Rare earth elements are widely used in the electronics industry, permanent magnets, luminescent materials, catalysts and other fields, and are important raw materials for high-tech industries (N. Zhang, S. Salzinger, F. Deubel, R. Jordan, B. Rieger, Surface- initiated group transfer polymerization mediated by rare earth metal catalysts, J. Am. Chem. Soc. 2012, 134, 7333-7336). However, the relevant treatment technology is not yet perfect, and people are concerned about the low concentration of rare earth and a large number of non-lanthanide competitive ions (such as Al in rare earth tailings or rare earth waste). 3+ , Fe 3+ etc.) are often easily overlooked, and the similar physical and chemical properties between rare earth element ions increase the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/30G01N21/64C09K11/06
CPCC08G83/008B01J20/226G01N21/643C09K11/06C09K2211/182Y02P10/20
Inventor 邱建丁宋安敏梁汝萍
Owner NANCHANG UNIV
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