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Method for synthesizing sulfydryl functionalized metal-organic framework MIL-101-SH through post-modification method

An organic framework and functionalization technology, which is used in the synthesis of thiol-functionalized metal-organic framework MIL-101-SH, can solve the problems of low adsorption capacity, limited application, and limited adsorption capacity.

Inactive Publication Date: 2019-03-22
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since metal-organic frameworks have only a few unsaturated sites, the adsorption capacity of metal-organic frameworks for heavy metal ions is greatly limited, and the adsorption capacity of metal-organic frameworks for heavy metal ions is not high, which greatly Limiting the application of metal-organic frameworks as adsorbents for heavy metal ions

Method used

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  • Method for synthesizing sulfydryl functionalized metal-organic framework MIL-101-SH through post-modification method
  • Method for synthesizing sulfydryl functionalized metal-organic framework MIL-101-SH through post-modification method
  • Method for synthesizing sulfydryl functionalized metal-organic framework MIL-101-SH through post-modification method

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Experimental program
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Effect test

Embodiment 1

[0057]1.1. Weigh 400mg of chromium nitrate nonahydrate, 181mg of 2-aminoterephthalic acid and 100mg of sodium hydroxide, add to 7.5mL of deionized water, sonicate until completely dissolved, and transfer the mixture to a high-pressure container with a polytetrafluoroethylene liner. React in an oven at 150°C for 12 hours in a reaction kettle. After the reaction is completed, take it out of the oven, cool to room temperature and collect the solid by centrifugation, and wash the solid several times with N,N-dimethylformamide to obtain the amino functionalized metal-organic framework Cr-MIL-101-NH 2 .

[0058] 1.2. Add 19.5mL of chloroacetaldehyde to 58.8mL of deionized water at zero degrees Celsius under ice bath conditions, and adjust the pH value to about 3 with sodium carbonate solution; under ice bath conditions, completely dissolve 5.6g of sodium hydrosulfide in 33mL deionized water at zero degrees Celsius; add sodium hydrosulfide solution to chloroacetaldehyde solution, st...

Embodiment 2

[0062] 2.1. Disperse 1350.0mg of ferric chloride hexahydrate in 15mL of N,N-dimethylformamide, then dissolve 450.0mg of 2-aminoterephthalic acid in 15mL of N,N-dimethylformamide, and After the two solutions were fully mixed, they were transferred to a high-pressure reactor with a polytetrafluoroethylene liner, and reacted at 110° C. for 20 hours. After the reaction is completed, wash the solid with N,N-dimethylformamide to obtain Fe-MIL-101-NH 2 .

[0063] 2.2. Weigh 290mg Fe-MIL-101-NH 2 Mix it with 76mg of mercaptoacetaldehyde in methanol, heat and keep the temperature at 65°C in an oil bath, condense and reflux, and react for 24 hours under magnetic stirring conditions. After the reaction was completed, the solid was collected by centrifugation, and the solid was washed several times with methanol to obtain the mercapto functionalized metal-organic framework Fe-MIL-101-SH.

Embodiment 3

[0065] 3.1. Dissolve 272mg of 2-aminoterephthalic acid in 60mL of N,N-dimethylformamide and heat to 110°C in an oil bath. Divide 724mg of aluminum trichloride hexahydrate into seven equal portions and add to the above solution, with an interval of 15 minutes between two times. Continue magnetic stirring for 3 hours after the last addition, and continue to react at 110°C for 16 hours after the stirring is stopped. After the reaction is completed, wash the solid with N,N-dimethylformamide and ethanol to obtain Al-MIL-101- NH 2 .

[0066] 3.2. Weigh 230mg Al-MIL-101-NH 2 Mix it with 76mg of mercaptoacetaldehyde in methanol, heat and keep the temperature at 65°C in an oil bath, condense and reflux, and react for 24 hours under magnetic stirring conditions. After the reaction was completed, the solid was collected by centrifugation, and the solid was washed several times with methanol to obtain the mercapto functionalized metal-organic framework Al-MIL-101-SH.

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Abstract

The invention discloses a method for synthesizing a sulfydryl functionalized metal-organic framework MIL-101-SH through a post-modification method and belongs to the technical field of synthesis of crystalline state materials and heavy metal ion adsorbents in water bodies. The method comprises the following synthesizing steps: (1) synthesizing an amino functionalized metal-organic framework MIL-101-NH2 through a solvothermal method; (2) reacting the amino functionalized metal-organic framework MIL-101-NH2 with mercaptoacetaldehyde through the post-modification method to synthesize the sulfydryl functionalized metal-organic framework MIL-101-SH. The sulfydryl functionalized metal-organic framework MIL-101-SH can be used as an adsorbent to be applied to adsorbing and removing heavy metal ions in water bodies; adsorption data show that the MIL-101-SH can well adsorb and remove mercury ions; compared with MIL-101-NH2, the adsorption performance is remarkably improved. In addition, the MIL-101-SH can selectively adsorb and remove mercury ions.

Description

technical field [0001] The invention belongs to the technical field of synthesis of heavy metal ion adsorbents in crystalline materials and water bodies, and in particular relates to a synthesis method of mercapto-functionalized metal-organic framework MIL-101-SH and its application in the field of adsorption and removal of heavy metal ions. technical background [0002] With the rapid development of my country's national economy, while improving people's quality of life, the problem of environmental pollution is becoming more and more prominent, among which heavy metal pollution is an extremely important environmental problem. Heavy metal ions mainly come from industrial wastewater and waste residues discharged from metallurgy, electrolysis, electroplating, storage batteries, chemicals, dyes and various mining processes. There are also a small amount of heavy metal ions in urban domestic sewage. [0003] At present, the commonly used methods for separation and removal of he...

Claims

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Application Information

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IPC IPC(8): B01J20/22C02F1/28B01J20/30C02F101/20
CPCB01J20/226C02F1/285C02F2101/20
Inventor 俞嘉梅王德超刘景昊王维吴玉锋
Owner BEIJING UNIV OF TECH
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