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Amidoxime group modified MOF material and preparation method thereof

A technology based on amidoxime and amidoxime, which is applied in the field of amidoxime-modified MOF materials and its preparation, can solve the problems of undiscovered MOF materials, expensive synthetic raw materials, and great impact on human health, and achieve selective adsorption The effect of good performance, fast adsorption rate and novel synthesis steps

Pending Publication Date: 2019-11-22
SOUTHWEAT UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, the processes of the above-mentioned prior art all carry out amidoxime group modification on the benzene ring, and no MOF material grafted with amidoxime group by coordinating ethylenediamine on the central Cr ion has been found, and the synthetic raw materials are expensive. , the solvent DMF used has serious environmental pollution and has a great impact on human health. DMF is listed in the list of 2A carcinogens
The product obtained by the predecessors has a low adsorption capacity for uranium and takes a long time to reach adsorption equilibrium

Method used

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  • Amidoxime group modified MOF material and preparation method thereof
  • Amidoxime group modified MOF material and preparation method thereof
  • Amidoxime group modified MOF material and preparation method thereof

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preparation example Construction

[0061] Preferably, the MIL-101(Cr) is prepared by the following method:

[0062] Fully disperse terephthalic acid and chromium nitrate nonahydrate in deionized water, then add mineralizer, and quickly package, at 200 ° C ~ 220 ° C, heat preservation reaction for 12 ~ 24 hours, purified to MIL-101 (Cr);

[0063] Wherein, the molar ratio of terephthalic acid, chromium nitrate nonahydrate and mineralizer is 4.8~5.0:4.8~5.0:2.0~4.0;

[0064] Preferably, the mineralizer is at least one of sodium acetate or hydrofluoric acid;

[0065] The mineralizer is preferably hydrofluoric acid, and the concentration of the hydrofluoric acid solution is preferably 40 wt%.

[0066] Preferably, the dehydration described in step (1) is:

[0067] Add dehydrating agent to MIL-101(Cr) to immerse MIL-101(Cr), oscillate ultrasonically for 2-4 hours, filter, wash with alcohol and deionized water alternately, and dry at 60-70°C for 12-24 hours;

[0068] The dehydrating agent is preferably at least one ...

Embodiment 1

[0079] (1) Preparation of MIL-101(Cr) with sodium acetate as a mineralizer: Weigh 0.01mol of terephthalic acid and 0.01mol of chromium nitrate nonahydrate, and disperse them in 80mL of 0.05mol / L sodium acetate solution in turn, Fully stir for half an hour, put it into a polytetrafluoroethylene-lined hydrothermal synthesis reactor at a temperature of 200° C., and keep it warm for 12 hours.

[0080] Naturally cool to room temperature after the reaction is completed, and then perform suction filtration. First, filter the turbid liquid with a medium-speed filter paper to remove most of the unreacted terephthalic acid, and then use a filter membrane with a pore size of 0.45 μm for suction filtration and deionized water and alcohol. Rinse alternately to remove terephthalic acid remaining on the surface and pores of MIL-101(Cr). The filtered product was dried in an oven at 70°C for 8 hours, and finally a pure green product MIL-101(Cr) was obtained.

[0081] (2) Activation of MIL-101...

Embodiment 2

[0088] (1) Preparation of MIL-101(Cr) with hydrofluoric acid as mineralizer: Weigh 0.01mol of terephthalic acid and 0.01mol of chromium nitrate nonahydrate, then disperse them into 50mL of deionized water, stir thoroughly for half an hour Put it into a hydrothermal synthesis reaction kettle with polytetrafluoroethylene lining, measure 0.20g of hydrofluoric acid solution with a mass fraction of 40%, quickly add it to the reaction kettle and package it quickly, then put it into a high-temperature oven, set the temperature At 220°C, keep warm for 14h. The suction filtration and drying operations are the same as the preparation of MIL-101 with hydrofluoric acid as mineralizer. Green MIL-101 (Cr) (hydrofluoric acid) was obtained after suction filtration and drying.

[0089] (2) Activation of MIL-101(Cr): Take an appropriate amount of MIL-101(Cr) and put them in a beaker for use, add an appropriate amount of N,N-dimethylformamide into the beaker to soak MIL-101(Cr) , Ultrasonic os...

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Abstract

The invention relates to an amidoxime group modified MOF material and a preparation method thereof, and belongs to the technical field of materials. The amidoxime group modified MOF material is an MIL-101(Cr) material, and a central atom of the MIL-101(Cr) material which is subjected to coordination modification by amidoxime groups is Cr. The amidoxime group modified MOF material has the advantages of large specific surface area, good water stability, high adsorption efficiency and high adsorption rate; has good selective adsorption performance on uranium, and has good application prospects inthe fields of seawater uranium extraction, radioactive wastewater treatment, environmental remediation and the like. The preparation method is simple in process and good in separation effect, terephthalic acid and chromic nitrate nonahydrate which are relatively cheap reagents are adopted, and the synthesis steps are novel.

Description

technical field [0001] The invention relates to an amidoxime-modified MOF material and a preparation method thereof, belonging to the field of material technology. Background technique [0002] The contradiction between energy and the environment in today's world is becoming increasingly prominent. Nuclear energy has been regarded as an important future energy source since its birth, and it has played a vital role in improving my country's energy structure, reducing the share of thermal power, and improving the environment. At present, my country's nuclear power industry mainly relies on the mining of terrestrial uranium ore, but my country's uranium ore is relatively scarce, and the development of the nuclear energy industry is limited. The reserves of uranium resources in the ocean are a thousand times that of terrestrial uranium resources. If properly developed, they can fully meet the leapfrog development of my country's nuclear energy industry. The key to extracting ur...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C22B3/24C22B60/02G21F9/12G21F9/20
CPCB01J20/226C22B3/24C22B60/0265G21F9/12G21F9/20
Inventor 匙芳廷曾毅杨李啸宇旦辉潘宁丁聪聪吴昊岩苟涵梁丹张爱
Owner SOUTHWEAT UNIV OF SCI & TECH
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