DMTD-COFs material as well as modification method and application thereof

A modification method and technology for adsorbing water, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc. The effect of increasing adsorption active sites, solving low adsorption capacity, and solving molecular diffusion problems

Active Publication Date: 2021-07-16
CHINA UNIV OF GEOSCIENCES (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention aims to solve the problem that the existing adsorption materials either have a low adsorption capacity for low-concentration heavy metals or require a long time for adsorption and diffusion

Method used

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  • DMTD-COFs material as well as modification method and application thereof
  • DMTD-COFs material as well as modification method and application thereof
  • DMTD-COFs material as well as modification method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) 2,5-divinyl terephthalaldehyde (Dva, 22.3mg, 0.12mmol), 1,3,5-tris(4-aminophenyl)benzene (Tab, 28.1mg, 0.08mmol), Add 0.1ml 6M acetic acid, 0.5ml n-butanol, and 0.5ml 1,2-dichlorobenzene to the 5ml ampoule in sequence. Put the ampoule in liquid N 2 Rapid freezing in the bath, vacuuming, liquid nitrogen freezing-pumping-thawing three times, vacuumize the ampoule, and seal the ampoule with a flame spray gun. The ampoule was reacted at 100°C for 3 days to obtain a yellow-brown precipitate, which was separated by filtration and washed with anhydrous tetrahydrofuran in a Soxhlet extractor for 2 days. The product was dried under vacuum at 50 °C to obtain COFs containing C=C double bonds.

[0052] (2) Under the condition of 80℃ water bath, under N 2 0.1079 g of DMTD was dissolved in 2 ml of ethanedithiol (the molar ratio of ethanedithiol to DMTD was 34:1) under atmosphere. in N 2 Under the atmosphere, the above solution was added to a 25ml Schleck tube containing 50mg...

Embodiment 2

[0070] Carry out application test to DMTD-COFs material of the present invention:

[0071] (1) The COFs prepared in 10mg embodiment 1 and the DMTD-COFs sample prepared when the molar ratio of ethanedithiol and DMTD was 34:1 were added to the Pb containing 30ml 2+ Concentration of 400ppb, Ca hardness of 20ppm, pH = 6.5 ± 0.25 solution in the Erlenmeyer flask. After oscillating at a constant temperature in a water bath at 20°C for 5 minutes, take 5.00ml for centrifugation, pass the supernatant through a 0.22μm filter membrane, add 1% nitric acid to acidify and make the volume to 10.00ml, and measure Pb in the solution by ICP-MS 2+ Concentration, the measurement result is multiplied by the dilution factor 2 to get the actual Pb in the solution 2+ concentration. In this way, the adsorption performance of DMTD-COFs was evaluated and compared with unmodified COFs.

[0072] Figure 8 The adsorption properties of DMTD-COFs samples prepared when the molar ratio of ethanedithiol to ...

Embodiment 3

[0083] (1) 2,5-divinyl terephthalaldehyde (Dva, 22.3mg, 0.12mmol), 1,3,5-tris(4-aminophenyl)benzene (Tab, 28.1mg, 0.08mmol), Add 0.1ml 6M acetic acid, 0.5ml n-butanol, and 0.5ml 1,2-dichlorobenzene to the 5ml ampoule in sequence. Put the ampoule in liquid N 2 Rapid freezing in the bath, vacuuming, liquid nitrogen freezing-pumping-thawing three times, vacuumize the ampoule, and seal the ampoule with a flame spray gun. The ampoule was reacted at 100°C for 3 days to obtain a yellow-brown precipitate, which was separated by filtration and washed with anhydrous tetrahydrofuran in a Soxhlet extractor for 2 days. The product was dried under vacuum at 50 °C to obtain COFs containing C=C double bonds.

[0084] (2) Under the condition of 80℃ water bath, under N 2 0.0540 g of DMTD was dissolved in 2 ml of ethanedithiol (the molar ratio of ethanedithiol to DMTD was 68:1) under atmosphere. in N 2 Add this solution under atmosphere to the 25ml Schlek tube (the mass ratio of DMTD, COFs ...

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Abstract

The invention relates to a DMTD-COFs material as well as a modification method and application thereof, in particular to a DMTD-COFs material capable of efficiently adsorbing low-concentration heavy metals in water as well as a modification method and application thereof, and belongs to the technical field of material modification and drinking water deep purification. The DMTD-COFs material capable of efficiently adsorbing the low-concentration heavy metal in the water is obtained by grafting 2, 5-dimercapto-1, 3, 4-thiadiazole on a COFs material. The modification method comprises the following steps: dissolving DMTD in dithioglycol under heating and inert atmosphere; in an inert atmosphere, adding a DMTD-ethanedithiol solution into a Schlenk tube containing a COFs material and AIBN; keeping inert atmosphere, heating and stirring at constant temperature for reaction; washing a solid sample with an organic solvent; and carrying out vacuum drying on the solid sample. The material can quickly and efficiently adsorb low-concentration heavy metals in water, and is large in adsorption capacity and good in adsorption selectivity.

Description

technical field [0001] The present invention relates to a DMTD-COFs material and its modification method and application, in particular to a DMTD-COFs material capable of efficiently adsorbing low-concentration heavy metals in water and its modification method and application, including the use of 2,5-dimercapto -1,3,4-Thiadiazole (DMTD) modified COFs materials containing double bonds to obtain DMTD-COFs materials, modification methods and the deep purification of low-concentration heavy metals in water, which belong to material modification and drinking The technical field of deep water purification. The present invention uses DMTD to modify COFs materials containing double bonds to add more active sites for adsorption, and exert the strong affinity of sulfur and nitrogen for heavy metals to enhance the affinity between materials and micro / trace heavy metals and overcome Mass transfer resistance, thereby greatly improving the ability and rate of materials to capture heavy me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F101/20
CPCB01J20/226B01J20/22C02F1/285C02F2101/20
Inventor 郑红杨雅喃张煜
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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