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Synthesis and adsorption application of alkali-resistant halogen bond donor metal organic framework

A metal-organic framework, alkali-resistant technology, applied in the directions of radioactive purification, greenhouse gas reduction, climate sustainability, etc., to achieve the effects of environmental friendliness, economic efficiency, increase adsorption capacity, and improve chemical stability

Pending Publication Date: 2022-07-12
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, no halogen bond donor metal-organic frameworks have been found to remove ReO by adsorption under strong alkali conditions. 4 - / 99 TCO 4 - report

Method used

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  • Synthesis and adsorption application of alkali-resistant halogen bond donor metal organic framework
  • Synthesis and adsorption application of alkali-resistant halogen bond donor metal organic framework
  • Synthesis and adsorption application of alkali-resistant halogen bond donor metal organic framework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Preparation and characterization of alkali-resistant halogen bond donor metal-organic framework (Mn-MOF)

[0036] Mix 0.0225 g of nitrogen-containing neutral ligand tris(4-(1H-imidazol-1-yl)phenyl)amine (Tipa) and 0.0396 g of MnCl 2 ·4H 2 O placed in a polytetrafluoroethylene reaction kettle, then added 3.5mL of N,N-dimethylformamide (DMF) and 40uL of concentrated hydrochloric acid, mixed evenly to obtain a reaction mixture; sealed the reaction kettle, placed it in After reacting at 120 °C for 3 days in an oven, it was cooled to room temperature at a rate of 5 °C / h to obtain a reaction product solution; the reaction product solution was taken out and filtered, and the crystals were washed with N,N-dimethylformamide and anhydrous ethanol. The crystals are placed in the air to dry to obtain alkali-resistant halogen bond donor metal organic framework Mn-MOF.

[0037] figure 1 is the crystal structure diagram of Mn-MOF. The crystal structure of Mn-MOF was mea...

Embodiment 2

[0039] Example 2: Mn-MOF versus ReO 4 - adsorption

[0040] (1) pH optimization

[0041] to ReO 4 - The pH of the solution was optimized. Add 10 mg of Mn-MOF to 10 mL of ReO containing 200 mg / L 4 - solution, with HNO 3 or NaOH to adjust the pH value of the solution (3,4,5,6,7,8,9,10,11,12,13), shake on a shaker for 12h at room temperature, filter with a 0.22μm membrane filter, and pass the inductively coupled plasma Determination of Residual ReO in Filtrate by Mass Spectrometry 4 - Concentration, Calculated Mn-MOF vs ReO 4 - removal rate. The results show that Mn-MOF is effective for ReO in the pH range of 4-12. 4 - The adsorption and removal efficiency of Mn-MOF is about 90%. 4 - The removal efficiency was 94.9%.

[0042] (2) Mn-MOF to ReO 4 - The adsorption capacity and adsorption kinetic behavior of

[0043] Dissolve sodium perrhenate in deionized water to prepare perrhenate solutions of different concentrations (10-1000mg / L), use HNO 3 or NaOH to adjus...

Embodiment 3

[0047] Example 3: The effect of Mn-MOF on ReO under strong alkaline conditions 4 - removal performance

[0048] Different mass (5mg, 12.5mg, 25mg, 50mg, 100mg) of Mn-MOF was added to 5mL of ReO containing 100mg / L 4 - 1M NaOH solution, shake the mixture at room temperature for 12h, take 1mL of the mixture and filter it with a 0.22μm membrane filter, and detect the residual ReO in the filtrate by inductively coupled plasma mass spectrometry 4 - concentration, calculating the effect of Mn-MOF on ReO under strong alkaline conditions 4 - removal rate. Figure 8 is the effect of Mn-MOF on ReO under 1M NaOH 4 - removal efficiency. Depend on Figure 8 It can be seen that in 1M NaOH, with the increase of solid-liquid ratio, ReO 4 - Mn-MOF can extract 90% of ReO at a solid-to-liquid ratio of 20 4 - , indicating that Mn-MOF is highly sensitive to ReO under strong alkaline conditions. 4 - high removal rate.

[0049] It can be seen that the alkali-resistant halogen bond do...

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Abstract

The invention discloses synthesis and adsorption application of an alkali-resistant halogen bond donor metal organic framework, and belongs to the technical field of environmental protection. The preparation method comprises the following steps: firstly, carrying out self-assembly positioning on MnCl2. 4H2O and a nitrogen-containing neutral ligand tri (4-(1H-imidazole-1-yl) phenyl) amine to generate a two-dimensional metal framework material (Mn-MOF) with alkali stability; a high-density metal halogen bond donor (Mn-Cl) in a Mn-MOF skeleton is combined with the anion ReO4 <-> through the action of a halogen bond, so that the adsorption capacity of the ReO4 <-> is greatly improved. A Mn-MOF skeleton contains a large number of one-dimensional hydrophobic channels constructed by benzene rings and imidazole rings, so that the Mn-MOF has higher affinity and selectivity to hydrophobic anions ReO4 <-> with small charge density than common competitive anions. The prepared Mn-MOF is high in stability in strong base, large in ReO4 <-> adsorption capacity, fast in dynamics and high in selectivity, and has good application potential.

Description

technical field [0001] The invention belongs to the technical field of environmental protection, and in particular relates to the synthesis and adsorption application of an alkali-resistant halogen bond donor metal organic framework. Background technique [0002] 99 Tc mainly comes from nuclear reactors 235 U and 239 Pu fission product. One ton of nuclear waste contains about 600-1000 grams of Tc. During the long-term storage of high-level nuclear waste, due to its long half-life (2.13×10 5 years) and a fission yield of up to 6%, making it extremely harmful to the environment (E.A.Katayev, G.V.Kolesnikov, J.L.Sessler, Molecular recognition of pertechnetate and perrhenate, Chem.Soc.Rev.38(2009) 1572-1586 ). Considering the volatility of Tc(VII) complexes during high temperature vitrification, there is an urgent need to develop effective strategies to 99 Tc is removed from nuclear waste prior to vitrification. also, 99 Tc usually starts with 99 TcO 4 - exist in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/26G21F9/12
CPCC08G83/008B01J20/226G21F9/12Y02E30/30
Inventor 邱建丁胡清华梁汝萍
Owner NANCHANG UNIV