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Method for preparing carbon foam adsorbents modified by phenylboronic acid type metal organic framework materials

A metal-organic framework and phenylboronic acid-based technology, applied in organic chemistry, chemical instruments and methods, and other chemical processes, can solve problems such as poor selectivity, low reuse rate, and high cost

Inactive Publication Date: 2016-10-26
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods have their own unique advantages, they also have their own limitations. Among them, the common defects are poor selectivity, low reuse rate and huge cost.

Method used

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  • Method for preparing carbon foam adsorbents modified by phenylboronic acid type metal organic framework materials
  • Method for preparing carbon foam adsorbents modified by phenylboronic acid type metal organic framework materials
  • Method for preparing carbon foam adsorbents modified by phenylboronic acid type metal organic framework materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of carbon foam (CF)

[0033] Mix 3mL formaldehyde solution and 1.5mL melamine, then add 2g triethanolamine, then vigorously stir at 50°C and 500rpm for 20min, and then obtain a prepolymer solution. Then 6 mL of toluene solution was gradually added dropwise to the pre-poly solution, and then stirred at 1000 rpm for 2 min. The resulting emulsion was then polymerized at 60°C for 3 hours. Then dry it under vacuum at 50°C for 12 hours. 50 mg of the obtained high internal phase emulsion were fired in a tube furnace for 2 hours, and heated to 400, 500, and 600 degrees at 5°C / min to obtain CF-400, CF-500, and CF-600.

[0034] (2) Preparation of CF-500-B-MOF

[0035] First, put 50mg of CF-500 into 0.1g of zinc nitrate hexahydrate solution, and stir a mixed solution (v:v, 1:1) of 5mL of ethanol and water for 6 hours in a polytetrafluoroethylene reactor . Then add 40 mg of 3,5-dicarboxyphenylboronic acid (BBDC) and 40 mg of terephthalic acid (H 2 BDC) was rea...

Embodiment 2

[0037] (1) Preparation of carbon foam (CF)

[0038] 4mL of formaldehyde solution and 2mL of melamine were mixed, then 3g of triethanolamine was added, and then vigorously stirred at 500rpm at 70°C for 40min to obtain a prepolymer solution. Then gradually add 10 mL of toluene solution dropwise to the pre-poly solution, and then stir at 1000 rpm for 2 min. The resulting emulsion was then polymerized at 80°C for 5 hours. Then dry it under vacuum at 70 degrees for 48 hours. 50 mg of the obtained high internal phase emulsion were fired in a tube furnace for 2 hours, and heated to 400, 500, and 600 degrees at 5°C / min to obtain CF-400, CF-500, and CF-600.

[0039] (2) Preparation of CF-500-B-MOF

[0040] First, put 100mg of CF-500 into 0.2g of zinc nitrate hexahydrate solution and mix it with 15mL of ethanol and water (v:v, 1:1) and stir for 24 hours in a polytetrafluoroethylene reactor . Then add 50 mg of 3,5-dicarboxyphenylboronic acid (BBDC) and 50 mg of terephthalic acid (H ...

Embodiment 3

[0042] (1) Preparation of carbon foam (CF)

[0043] Mix 3.5mL formaldehyde solution and 2mL melamine, then add 2.5g triethanolamine, then stir vigorously at 60°C and 500rpm for 30min, and then obtain the prepolymer solution. Then 8 mL of toluene solution was gradually added dropwise into the pre-poly solution, and then stirred at 1000 rpm for 2 min. The resulting emulsion was then polymerized at 70°C for 4 hours. Then dry it under vacuum at 60°C for 24 hours. 50 mg of the obtained high internal phase emulsion were fired in a tube furnace for 2 hours, and heated to 400, 500, and 600 degrees at 5°C / min to obtain CF-400, CF-500, and CF-600.

[0044] (2) Preparation of CF-500-B-MOF

[0045] First, put 75mg of CF-500 into 0.15g of zinc nitrate hexahydrate solution and stir for 12 hours in a mixed solution (v:v, 1:1) composed of 10mL of ethanol and water in a polytetrafluoroethylene reactor . Then add 45 mg of 3,5-dicarboxyphenylboronic acid (BBDC) and 45 mg of terephthalic aci...

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Abstract

The invention belongs to the field of technologies for preparing environment functional materials, and particularly discloses a method for preparing carbon foam adsorbents modified by phenylboronic acid type metal organic framework materials. The method includes synthesizing high-temperature-resistant high-internal-phase materials; calcining the high-temperature-resistant high-internal-phase materials in a tube furnace to obtain carbon foam; soaking carbon foam materials in zinc ion solution; adding an organic ligand (terephthalic acid) and a ligand fragment (3, 5-dicarboxy phenylboronic acid) into the zinc ion solution and carrying out a series of treatment to obtain the adsorbents; applying the adsorbents to selectively recognizing and separating luteolin. The method has the advantages that emulsion imprinted polymer micro-spheres prepared by the aid of the method are high in heat stability, the luteolin can be efficiently adsorbed, and the carbon foam adsorbents have acid-alkali control release performance.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of environmental functional materials, and relates to a method for modifying carbon foam adsorbents with phenylboronic acid-type metal-organic framework materials. Background technique [0002] Macroporous materials have attracted extensive attention due to their remarkable compression resistance and have been used in many fields, such as catalysts, tissue engineering, adsorption and separation, etc.; the traditional method of preparing such macroporous materials is to polymerize them with surfactants. High internal phase emulsion (High Internal Phase Emulsion, HIPE), also known as high-concentration emulsion, is an emulsion with a dispersed phase volume fraction greater than 74.05%. [0003] Metal-organic frameworks are three-dimensional porous materials formed by the self-assembly of organic ligands and metal ions or clusters through coordination bonds. Due to its huge specific surface are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/32C07D311/30
CPCB01J20/205B01J20/223B01J20/3204B01J2220/46B01J2220/4812C07D311/30
Inventor 刘树成潘建明夏大厦姚俊彤黄伟
Owner JIANGSU UNIV
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