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Covalent organic framework material containing sulfonic acid groups as well as preparation and application of covalent organic framework material

A covalent organic framework and sulfonic acid group technology, applied in the fields of environmental protection and resource recycling, can solve the problems of poor effect, slow ammonia nitrogen adsorption rate, and low adsorption capacity, and achieve cost reduction, rapid separation capacity, and high The effect of adsorption capacity

Active Publication Date: 2021-04-20
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional adsorbents (such as zeolite, resin, etc.) have a slow adsorption rate and low adsorption capacity for ammonia nitrogen, especially for low-concentration ammonia nitrogen, and the performance is even worse.

Method used

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  • Covalent organic framework material containing sulfonic acid groups as well as preparation and application of covalent organic framework material
  • Covalent organic framework material containing sulfonic acid groups as well as preparation and application of covalent organic framework material
  • Covalent organic framework material containing sulfonic acid groups as well as preparation and application of covalent organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062]Example 1: Preparation of a covalent organic frame polymer (TPBSA-1) containing a sulfonic acid group

[0063]63 mg (0.3 mmol) 1,3,5-trialdehyde-based benzene (TP) and 84.69 mg (0.45 mmol) 2,5-diaminophenylsulfonic acid (BSA-1) were added to the custom test tube, respectively. Then, 1.5 ml of 10 ml 1,4-dioxane, 0.5 ml of 3 mol / L of acetic acid solution was then added and ultrasonic 10min, and the reactant and solvent were sufficiently mixed; The liquid nitrogen is frozen, and the step of vacuuming, degassing, and thawing is repeated 3 times to ensure that the solvent is no longer bubbles; using the aluminum spray light to fusion, finally put the test tube in an oven at 120 ° C for 3 days After the reaction, the centrifugal filtration can be dull red, and the precipitate was washed 5 to 6 times with acetone and DMF, and then the solvent was cleaned with the solvent; finally was placed in a vacuum drying tank for 24 h in a vacuum drying tank. The organic covalent frame polymer (T...

Embodiment 2

[0064]Example 2: Preparation of a covalent organic frame polymer (TPBSA-2) containing a sulfonic acid group

[0065]63 mg (0.3 mmol) 1,3,5-trialdehyde-based benzene phenol (TP) and 120.72 mg (0.45 mmol) 2,5-diaminophenyl-1,4-disulfonic acid (BSA-2) Added to the custom test tube, then 1.5 ml of tetrahydrobenzene, 1.5 ml 1,4-dioxane, 0.5 ml of 3 mol / L of acetic acid solution and ultrasonic 10min, so that the reactants and solvents are sufficiently mixed; After connecting the vacuum device, it is frozen in liquid nitrogen, and repeated three times in the step of vacuuming, degassing, and thawing. Ensuring no bubbles are generated; using alcohol spray light to vacuum, finally place the test tube in 120 The reaction was reacted for 3 days; after the reaction was completed, the centrifugal filtration was dark red, and the precipitate was washed with acetone and DMF, and the precipitate was cleaned with THF and washed several times in the solvent; finally placed red precipitate at 180 ° C i...

Embodiment 3

[0066]Example 3: Preparation of Covity Organic Frame Polymer (TPBDSA-1) containing a sulfonic acid group

[0067]63 mg (0.3 mmol) 1,3,5-trialdehyde-based phenol (TP) and 118.53 mg (0.45 mmol) 4,4'-diamino [1,1'-biphenyl] -3-sulfur The acid (BDSA-1) was added to the custom test tube, and then 1.5 ml of 10 ml 1,4-dioxane, 0.5 ml of 3 mol / L of acetic acid solution was added and ultrasonic 10min, and reactants and solvents Fully mixed; after the tube is connected to the vacuum device, it is frozen in liquid nitrogen, and repeated three times according to the step of vacuum, degassing, and thawing. Ensure that the solvent is no longer bubbles; using alcohol spray lamp to vacuum over the test tube. Finally, the test tube was placed in a 120 ° C oven reaction for 3 days; after the reaction, centrifugal filtration was dark red, washed with acetone and DMF 5 to 6 times, and then use THF for solvent to wash a few times; finally The precipitate was dried in a vacuum drying tank at 180 ° C, and ...

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Abstract

The invention relates to a covalent organic framework material containing a sulfonic acid group as well as preparation and application of the covalent organic framework material, a monomer 1, 3, 5-trialdehyde phloroglucinol and a sulfonic acid phenylenediamine monomer are subjected to a Schiff base reaction through a solvothermal method, and the TJU-COFs-SO3H covalent organic framework material containing the sulfonic acid group is finally prepared. The TJU-COFs-SO3H covalent organic framework material containing the sulfonic acid group is used for separating or recovering impurities or pollutants in water. Compared with the prior art, the TJU-COFs-SO3H provided by the invention introduces a sulfonic acid group, not only has the functions of ion exchange and the like, but also has a periodic pore structure and stable chemical characteristics, and compared with COFs without the sulfonic acid group, the TJU-COFs-SO3H has better performance of separating cations in water, especially for separating low-concentration ammonia nitrogen, and can be used for separating the cations in water. The TJU-COFs-SO3H covalent organic framework material has the characteristics of ultra-high rate, high adsorption capacity, reusability and the like, and also has similar effects on other cations in water, such as metal ions and the like.

Description

Technical field[0001]The present invention belongs to the field of environmental protection and resource recovery, and more particularly to a covalent organic frame material containing a sulfonic acid group and its preparation and application thereof.Background technique[0002]Nitrogen is an important agricultural production resource, mainly through the Haber-Bosch craftsmanship, which is estimated to consume 12.1 kWh energy per kilograms of ammonia, and the cost of approximately 1.5 US dollars, about 100 million nitrogen fertilizers per year. There are about 2 million tons world every year, and it is expected to increase to 35 million tons of active nitrogen by 2050, and emissions into the water body.[0003]Compared to some industries, such as industrial enterprises such as nitrogen, high-concentration ammonia nitrogen wastewater, ammonia nitrogen concentration, and economical recovery value, and low-alcoht nitrogen concentration in the source of pollution and water sewage, and rough...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/02B01J20/22C02F1/28
CPCY02W10/10
Inventor 金伟黄乃先刘静林徐祖信李怀正齐一凡
Owner TONGJI UNIV
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