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Microwave synthesized metal organic framework material DUT-5 (Al) as well as synthesis method and application thereof

A metal-organic framework and DUT-5 technology, which is applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problems of long time consumption and low efficiency, so as to improve adsorption efficiency and synthesis Efficiency, the effect of shortening the synthesis time

Pending Publication Date: 2021-12-28
QINGDAO AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional synthesis method of MOF is hydrothermal / solvothermal method, but this method is time-consuming and inefficient. Therefore, an efficient and controllable method is needed to synthesize MOFs, and currently few MOFs are used to remove PFOS and PFOA from water. public report

Method used

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  • Microwave synthesized metal organic framework material DUT-5 (Al) as well as synthesis method and application thereof
  • Microwave synthesized metal organic framework material DUT-5 (Al) as well as synthesis method and application thereof
  • Microwave synthesized metal organic framework material DUT-5 (Al) as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: the synthesis of MOFs

[0032] Synthesis of MOFs by hydrothermal / solvothermal method or microwave-assisted synthesis, the schematic diagram of material synthesis can be found in figure 1 .

[0033] 1. Synthesis of UIO-66

[0034] The traditional solvothermal synthesis method was adopted. According to n (ZrCl 4 ): n (terephthalic acid) = 1:1 ratio, 2.33g zirconium tetrachloride (Zrcl 4 ) and 1.66g terephthalic acid (H 2 BDC) was dissolved in 200mL N,N-dimethylformamide (DMF), stirred until dissolved and loaded into a polytetrafluoroethylene reactor (15.5*7.70 cm, Shanghai Wutong Experimental Instrument Co., Ltd.), at 120°C Under reaction 24h. The product was washed 3 times with DMF and methanol respectively and collected by centrifugation. Finally, the product was dried in a vacuum oven at 120°C for 8 hours to obtain metal-organic framework material UIO-66 crystal, and the UIO-66 crystal powder was sealed and stored for future use.

[0035] 2. Synth...

Embodiment 2

[0047] Embodiment 2: the screening of adsorbent

[0048] To evaluate the synthesized MOFs (DUT-5-1, DUT-5-2, UIO-66, UIO-67, MOF-801, NH 2 -MIL-101 and Co-MOF) on the adsorption performance of PFOS and PFOA, the static adsorption experiment was carried out. Specifically: Add 5 mg of adsorbent to a 50 mL polypropylene centrifuge tube containing 25 mL of PFOS or PFOA solution with a concentration of 30 mg / L. Before adding the adsorbent, add 0.1 mol / L HCl or NaOH Solution Adjust the pH of the PFOS or PFOA solution to 3.0±0.1. These mixtures were placed in a constant temperature shaker (25°C) and shaken at a speed of 150 r / min for 24 h. Samples were taken and filtered with a 0.22 μm filter membrane, and the concentrations of PFOS and PFOA in the solution were determined after filtration. And calculate the adsorption capacity according to formula (1).

[0049] Formula 1);

[0050] Among them: C 0 —Initial concentration of PFOS or PFOA (mg / L);

[0051] C t - remaining con...

Embodiment 3

[0056] Example 3: Research on the Adsorption Behavior of DUT-5-2 to PFOS and PFOA

[0057] 1. Morphology and structure characterization of DUT-5-2

[0058] (1) Scanning electron microscope (SEM) and Zeta potential analysis

[0059] The surface morphology of metal-organic frameworks was observed using a JEOL 7500F scanning electron microscope (SEM). The obtained sample powder was fixed on a stainless steel sample stage with conductive glue, and a layer of gold was sprayed on the surface to avoid electron beam charging. The gold-sprayed sample was placed under a scanning electron microscope at 2.00 KV to observe the surface microstructure of the metal-organic framework.

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Abstract

The invention discloses a microwave synthesized metal organic framework material DUT-5 (Al) as well as a synthesis method and application thereof. The method comprises the following steps: dissolving diphenyldicarboxylic acid in N, N-dimethylformamide, adding Al(NO3)3.9H2O, uniformly stirring, carrying out microwave reaction on the mixed solution, cooling the reaction solution after the reaction is finished, centrifugally collecting the precipitate, washing and drying to obtain the metal organic framework material DUT-5 (Al). According to the microwave synthesis of the DUT-5 (Al), the synthesis time is greatly shortened, the synthesis efficiency is improved, the adsorption efficiency of the DUT-5 (Al) on PFOS and PFOA is obviously improved, the DUT-5 (Al) can be recycled for more than four times, and the adsorption regeneration rate of the DUT-5 (Al) on the PFOS and PFOA in a water environment reaches more than 90%, so that the DUT-5 (Al) has a wide application prospect.

Description

technical field [0001] The invention belongs to the field of adsorbent materials, and in particular relates to a microwave-synthesized metal-organic framework material DUT-5(Al) and its synthesis method and application. Background technique [0002] Perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) are generally considered to be the most representative perfluorinated and polyfluoroalkyl substances (PFAS). Due to its unique hydrophobic and lipophobic physical and chemical properties, it has been widely used in surfactants, insecticides, fire fighting foams and industrial production. PFOS and PFOA are persistent, bioaccumulative, toxic, and even potentially carcinogenic. PFOS and PFOA pose potential threats to the ecological environment and human health. PFOS and its salts, PFOA and its salts, and compounds related to PFOA have all been included in the Stockholm Convention. And according to the requirements of the Ministry of Ecology and Environment of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22C02F1/28B01J20/30C02F101/36
CPCB01J20/226C02F1/285C02F2101/36
Inventor 张双灵郭萌萌胡月戴振建姜文利薛长晖杜德红王丽东野子璇
Owner QINGDAO AGRI UNIV
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