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A kind of preparation method and application of cross-linked resin after imidazole modification

A cross-linked resin and imidazole technology, applied in the field of functional polymer synthesis, can solve the problems of unsatisfactory adsorption performance of polar organic substances in water, etc., and achieve the effect of improving adsorption performance, improving pore structure, and good selective adsorption

Inactive Publication Date: 2018-01-09
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defect that the existing post-crosslinking resin has unsatisfactory adsorption performance to polar organic substances in water, the purpose of the present invention is to provide a preparation with high specific surface area and large pore volume, and has suitable pore structure and polarity, especially A method for a novel imidazole-modified post-crosslinked resin suitable for adsorbing polar small molecule aromatic organic compounds in water, the method is simple to operate and low in cost, and can meet industrial production requirements

Method used

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  • A kind of preparation method and application of cross-linked resin after imidazole modification
  • A kind of preparation method and application of cross-linked resin after imidazole modification
  • A kind of preparation method and application of cross-linked resin after imidazole modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) Preparation of precursor resin:

[0045] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. A mixture of 20 g of divinylbenzene (DVB) and 1-vinylimidazole (VIM), a mixed solvent of 40 g of o-xylene and benzyl alcohol, and 0.2 g of azobisisobutyronitrile (AIBN) were added. Heat to 45°C, adjust to a suitable stirring speed and stir for 30min, raise the temperature to 75°C for 3h, raise the temperature to 85°C for 3h, continue to raise the temperature to 95°C for 3h. After cooling, alternately wash the resin with absolute ethanol, hot water, and cold water until the washing solution is clear, extract it with petroleum ether in a Soxhlet extractor for 12 hours, and dry it in vacuum for 24 hours to obtain the precursor resin PDV-90%-0%, PDV-90%-25% and PDV-90%-100%.

[0046] 2) Friedel-Crafts reaction:

[0047] Add 15g of precursor resins PDV-90%-0%, PDV-90%-25% and PDV-90%-100% and 50mL 1...

Embodiment 2

[0054] 1) Preparation of precursor resin:

[0055]Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. Add 20g of a mixture of divinylbenzene (DVB) and 2-methyl-1-vinylimidazole (MVIM); 60.0g of a mixed solvent of o-xylene and benzyl alcohol, and 0.2g of azobisisobutyronitrile (AIBN). Heat to 45°C, adjust to an appropriate stirring speed and stir for 30 minutes, raise the temperature to 68°C for 5 hours, raise the temperature to 78°C for 5 hours, and continue to heat up to 90°C for 5 hours. After cooling, alternately wash the resin with absolute ethanol, hot water, and cold water until the washing solution is clear, extract it with petroleum ether in a Soxhlet extractor for 12 hours, and dry it in vacuum for 24 hours to obtain the precursor resin PDMV-95%-20%, PDMV-85%-50% and PDMV-70%-80%.

[0056] 2) Friedel-Crafts reaction:

[0057] Add 15g of precursor resins PDMV-95%-20%, PDMV-85%-50% and PD...

Embodiment 3

[0064] 1) Preparation of precursor resin:

[0065] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. A mixture of 20 g of divinylbenzene (DVB) and 2-ethyl-1-vinylimidazole (EVIM), a mixed solvent of 20.0 g of o-xylene and benzyl alcohol, and 0.2 g of azobisisobutyronitrile (AIBN) were added. Heat to 45°C, adjust to an appropriate stirring speed and stir for 30 minutes, raise the temperature to 68°C for 5 hours, raise the temperature to 78°C for 5 hours, and continue to heat up to 90°C for 5 hours. After cooling, alternately wash the resin with absolute ethanol, hot water, and cold water until the washing liquid is clear, extract it with petroleum ether in a Soxhlet extractor for 12 hours, and dry it in vacuum for 24 hours to obtain the precursor resin PDEV-90%-90%, PDEV-80%-60% and PDEV-70%-30%.

[0066] 2) Friedel-Crafts reaction:

[0067] Add 15g of precursor resins PDEV-90%-90%, PDEV-80%-60...

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Abstract

The invention discloses a preparation method and application of cross-linked resin modified by imidazole. The preparation method of cross-linked modified by imidazole comprises the steps that a vinyl-containing imidazole monomer, a divinylbenzene cross-linking agent, an initiator, an o-xylene and / or benzyl alcohol pore-forming agent and a dispersing agent are subjected to suspension polymerization to obtain precursor resin; the precursor resin is subjected to a Friedel-Crafts reaction under the Lewis acid catalytic action, and the cross-linked resin modified by imidazole with the high specific surface area, large pore volume and the proper pore structure and polarity is obtained. The resin is particularly applicable to adsorbing small polar molecular aromatic organic compounds in water. In addition, the preparation method of the cross-linked resin modified by imidazole is simple, low in cost and capable of achieving industrial production.

Description

technical field [0001] The invention relates to a preparation method and application of a post-crosslinking resin, in particular to a preparation method and application of an imidazole-modified post-crosslinking resin, and belongs to the technical field of functional polymer synthesis. Background technique [0002] In the early 1970s, Davankov et al cross-linked linear polystyrene or low-crosslinked polystyrene through the Friedel-Crafts reaction to form a class of porous polymers with unique structures and excellent properties. Higher degree, also known as post-crosslinking resin. Post-crosslinked resins usually have structural characteristics such as large specific surface area, small average pore size, narrow pore size distribution, and good mechanical strength. At present, they have shown broad application prospects in the treatment of toxic organic wastewater, gas storage and separation, and other fields. Chloromethyl methyl ether is often used as the chloromethylation...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F226/06C08F212/36C08F8/02C08F2/20C08J9/28B01J20/26B01J20/30
CPCB01J20/267C08F2/20C08F8/02C08F226/06C08J9/28C08J2339/04C08F212/36
Inventor 黄健涵伏振宇董建洋刘又年邵礼书张婷刘明强梁成易承志
Owner CENT SOUTH UNIV
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