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Preparation method of heavy metal ion adsorbent based on amino functionalized silsesquioxane

A technology of silsesquioxane and heavy metal ions, applied in chemical instruments and methods, other chemical processes, improvement of process efficiency, etc., can solve the problems of low adsorption capacity of heavy metal ions, insufficient research, etc., and meet the preparation process conditions Ease of control, ease of raw materials, and high yield

Active Publication Date: 2021-04-16
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the research on network functional materials based on cage-type silsesquioxanes is not enough, and the adsorption capacity of heavy metal ions is not high; the network functional materials obtained by hydrophilically modifying cage-type silsesquioxanes are expected to show some more superior properties, so this research is very necessary

Method used

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  • Preparation method of heavy metal ion adsorbent based on amino functionalized silsesquioxane
  • Preparation method of heavy metal ion adsorbent based on amino functionalized silsesquioxane
  • Preparation method of heavy metal ion adsorbent based on amino functionalized silsesquioxane

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Embodiment 1

[0042] A preparation method based on amino functionalized silsesquioxane heavy metal ion adsorbent (having the structure shown in PAC-1), the steps are as follows:

[0043] The octachloropropyl silsesquioxane of 0.73g (0.7mmol) cage structure, 0.32g (2mmol) triaminoethylamine are packed in the dry three-necked flask that has condenser and magnetic stirrer, flask Vacuumize and fill with nitrogen, then add 15mL N,N-dimethylformamide (DMF), stir the mixture at room temperature for 2 hours, after dissolving completely, add 7mL triethylamine, continue to stir for 3h and mix well, then raise the temperature to 110 ℃. The reaction was stirred at 110°C for 24 hours. After the reaction, cool to room temperature, filter to obtain a solid polymer, wash the solid polymer with acetone, water, absolute ethanol and dichloromethane successively for 3 times, then perform Soxhlet extraction with ethanol for 72 hours, and vacuum-dry at 70°C for 24 hours , to obtain 0.95 g of brown-yellow powde...

Embodiment 2

[0051] A preparation method based on amino functionalized silsesquioxane heavy metal ion adsorbent (having the structure shown in PAC-2), the steps are as follows:

[0052] The octachloropropyl silsesquioxane of 0.73g (0.7mmol) cage structure, 0.32g (2mmol) triaminoethylamine are packed in the dry three-necked flask that has condenser and magnetic stirrer, flask Vacuumize and fill with nitrogen, then add 15mL N,N-dimethylformamide (DMF), stir the mixture at room temperature for 2 hours and dissolve completely, add 1.07g sodium bicarbonate, continue to stir for 3h, mix well and then heat up to 110°C. The reaction was stirred at 110°C for 24 hours. After the reaction, cool to room temperature, filter to obtain a solid polymer, wash the solid polymer with acetone, water, absolute ethanol and dichloromethane successively for 3 times, then perform Soxhlet extraction with ethanol for 72 hours, and vacuum-dry at 70°C for 24 hours , to obtain 0.87 g of light yellow powdery solid (yi...

Embodiment 3

[0060] A preparation method based on amino functionalized silsesquioxane heavy metal ion adsorbent, the steps are as follows:

[0061] The octachloropropyl silsesquioxane of 0.73g (0.7mmol) cage structure, 0.32g (2mmol) triaminoethylamine are packed in the dry three-necked flask that has condenser and magnetic stirrer, flask Vacuum and fill with nitrogen, then add 20mL of N,N- dimethylformamide (DMF), stir the mixture at room temperature for 2 hours after dissolving completely, add 2ml of triethylamine, continue to stir for 3h and mix well, then raise the temperature to 110 ℃. The reaction was stirred at 110°C for 24 hours. After the reaction, cool to room temperature, filter to obtain a solid polymer, wash the solid polymer with acetone, water, absolute ethanol and dichloromethane successively for 3 times, then perform Soxhlet extraction with ethanol for 72 hours, and vacuum-dry at 70°C for 24 hours , that is.

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Abstract

The invention provides a preparation method of a heavy metal ion adsorbent based on amino functionalized silsesquioxane. The preparation method comprises the following steps: dissolving octachloropropyl silsesquioxane with a cage structure and triaminoethylamine in an organic solvent, adding an acid acceptor, uniformly mixing, and carrying out a heating reaction; after the reaction is finished, cooling to room temperature, filtering and washing to obtain a solid, wherein the acid acceptor is triethylamine or sodium bicarbonate; carrying out Soxhlet extraction on the obtained solid, and then drying to obtain the product. According to the invention, triethylamine or sodium bicarbonate is used as an acid acceptor, and two hybrid network functional material adsorbents with different structures are prepared through nucleophilic substitution reaction; the prepared adsorbent has good chemical stability and thermal stability, the adsorption capacity of the silsesquioxane-based hybrid material to heavy metal ions in wastewater is greatly improved, and the adsorbent has huge potential application value in the field of adsorption.

Description

technical field [0001] The invention relates to a preparation method of an amino functionalized silsesquioxane heavy metal ion adsorbent, which belongs to the technical fields of environmental protection and chemical separation. Background technique [0002] With the rapid development of the world economy, the machinery manufacturing industry has grown rapidly, but the environmental problems caused by it have become increasingly serious. Among them, the harm caused by the pollution of water resources has gradually intensified. Among the many pollutants, sudden heavy metal pollution is particularly serious. Heavy metals are refractory to degradation, and it is difficult to reduce their harmfulness only by the physical, chemical or microbial purification of water bodies. These reasons make it difficult for heavy metal pollution in water bodies to disappear after sudden heavy metal pollution accidents. For example, mercury has a strong bioaccumulation capacity, can enter and s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C08G77/26C08G77/24C08G77/06C02F101/20
CPCY02P10/20
Inventor 刘鸿志葛倩
Owner SHANDONG UNIV
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