A dmtd-cofs material and its modification method and application

A modification method and water adsorption technology, which is applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problems of low adsorption capacity of low-concentration heavy metals and long time required for adsorption and diffusion, and achieve Effects of increasing adsorption active sites, solving low adsorption capacity, and solving molecular diffusion problems

Active Publication Date: 2022-07-19
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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  • A dmtd-cofs material and its modification method and application
  • A dmtd-cofs material and its modification method and application
  • A dmtd-cofs material and its modification method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) 2,5-divinylterephthalaldehyde (Dva, 22.3 mg, 0.12 mmol), 1,3,5-tris(4-aminophenyl)benzene (Tab, 28.1 mg, 0.08 mmol), 0.1ml of 6M acetic acid, 0.5ml of n-butanol, 0.5ml of 1,2-dichlorobenzene were added sequentially to a 5ml ampoule. Place ampoules in liquid N 2 Quickly freeze under the bath, vacuumize, freeze-pump-thaw in liquid nitrogen three times, vacuumize the ampoule bottle, and seal the ampoule bottle with a flame spray gun. The ampoule was left to react 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, in 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 The above solution was added to a 25ml Schreek tube contain...

Embodiment 2

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

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

[0072] Figure 8 The adsorption performance of the DMTD-COFs samples prepared when the ...

Embodiment 3

[0083] (1) 2,5-divinylterephthalaldehyde (Dva, 22.3 mg, 0.12 mmol), 1,3,5-tris(4-aminophenyl)benzene (Tab, 28.1 mg, 0.08 mmol), 0.1ml of 6M acetic acid, 0.5ml of n-butanol, 0.5ml of 1,2-dichlorobenzene were added sequentially to a 5ml ampoule. Place ampoules in liquid N 2 Quickly freeze under the bath, vacuumize, freeze-pump-thaw with liquid nitrogen three times, vacuumize the ampoule bottle, and seal the ampoule bottle with a flame spray gun. The ampoule was left to react 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, in 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 The solution was added to a 25 ml Schreek tube containing...

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Abstract

The invention relates to a DMTD-COFs material and a modification method and application thereof, in particular to a DMTD-COFs material for efficiently adsorbing low concentrations of heavy metals in water, a modification method and application thereof, and belongs to the technical field of material modification and deep purification of drinking water. 2,5-dimercapto-1,3,4-thiadiazole was grafted on COFs materials to obtain DMTD-COFs materials that efficiently adsorbed low concentrations of heavy metals in water. The modification method is to dissolve DMTD in ethanedithiol under heating and inert atmosphere; under inert atmosphere, add DMTD-ethanedithiol solution to Schreek tube containing COFs material and AIBN; keep inert atmosphere , heating and stirring at constant temperature to carry out the reaction; using organic solvent to wash the solid sample; vacuum drying the solid sample. The material can quickly and efficiently adsorb low-concentration heavy metals in water, and has large adsorption capacity and good adsorption selectivity.

Description

technical field [0001] The invention relates to a DMTD-COFs material and a modification method and application thereof, in particular to a DMTD-COFs material capable of efficiently adsorbing low concentrations of heavy metals in water, and a modification method and application thereof, including the use of 2,5-dimercapto group containing rich functional groups The DMTD-COFs material obtained by modifying the double bond-containing COFs material with -1,3,4-thiadiazole (DMTD), the modification method and the deep purification of the low-concentration heavy metal in water by the material, belong to the material modification and drinking Water depth purification technology field. The invention uses DMTD to modify the double bond-containing COFs material to increase more adsorption active sites, exert the strong affinity of sulfur and nitrogen to heavy metals, so as to enhance the affinity between the material and micro / trace heavy metals, overcome the Mass transfer resistance, t...

Claims

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Application Information

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Patent Type & Authority Patents(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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