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Method for preparing polar modified ultrahighly-crosslinked resin and application of resin

An ultra-high cross-linked resin and polar technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems such as unsatisfactory adsorption effects, achieve content reduction, increase adsorption capacity, and improve pore structure. Effect

Inactive Publication Date: 2015-09-16
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the defect that the modified ultra-highly cross-linked polystyrene in the prior art has an unsatisfactory adsorption effect on polar organic substances in water (such as: weakly polar phenol, highly polar salicylic acid), making its application Restricted, the purpose of the present invention is to provide a preparation of high specific surface area and large pore volume, and has a suitable pore size and polar pore structure, especially suitable for the adsorption of polar small molecule aromatic organic compounds such as phenol and salicylic acid in water. The method for polar modification of ultra-high cross-linked resin, the method is simple to operate, low in cost, and satisfies industrial production

Method used

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  • Method for preparing polar modified ultrahighly-crosslinked resin and application of resin
  • Method for preparing polar modified ultrahighly-crosslinked resin and application of resin
  • Method for preparing polar modified ultrahighly-crosslinked resin and application of resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1) Preparation of ternary copolymerization precursor resin:

[0048] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. 1.0 g of oil phase divinylbenzene (DVB), 1.0 g of methyl acrylate (MA), 18.0 g of 4-vinylbenzyl chloride (VBC), 40.0 g of toluene, and 0.2 g of azobisisobutyronitrile (AIBN) were added. Heat to 45°C, adjust to a suitable stirring speed and stir for 30 minutes, raise the temperature to 75°C for 3 hours, raise the temperature to 85°C for 2 hours, and continue to raise the temperature to 95°C for 3 hours. After cooling, the resin was alternately washed with absolute ethanol, hot water, and cold water until the washing solution was clear, extracted with petroleum ether in a Soxhlet extractor for 12 hours, and dried in vacuum for 24 hours to obtain the ternary copolymerization precursor resin PVDM. The infrared characterization was as follows: figure 1 Shown, PVDM at 1263cm -...

Embodiment 2

[0057] 1) Preparation of ternary copolymerization precursor resin:

[0058] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. Added 2.0 g of divinylbenzene (DVB) oil phase, 2.0 g of methyl acrylate (MA), 16.0 g of 4-vinylbenzyl chloride (VBC), 50.0 g of toluene, and 0.2 g of benzoyl peroxide (BPO). Heat to 45°C, adjust to a suitable stirring speed and stir for 30 minutes, raise the temperature to 75°C for 3 hours, raise the temperature to 85°C for 2 hours, and continue to raise the temperature to 95°C for 3 hours. After cooling, alternately wash the resin with absolute ethanol, hot water, and cold water until the washing solution is clear, put it into a Soxhlet extractor and extract it with petroleum ether for 12 hours, and dry it in vacuum for 24 hours to obtain the ternary copolymerization precursor resin PVDM;

[0059] 2) Friedel-Crafts reaction:

[0060] Add 15g of ternary copolymerization ...

Embodiment 3

[0066] 1) Preparation of ternary copolymerization precursor resin:

[0067] Place a 500 mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer, and first add the water phase (180 mL of distilled water, 20 mL of polyvinyl alcohol with a mass fraction of 1%, 10 drops of methylene blue), and 1.5 g of divinylbenzene (DVB) oil phase, 1.5 g of ethyl acrylate (EA), 17.0 g of 4-vinylbenzyl chloride (VBC), 45.0 g of toluene, and 0.3 g of benzoyl peroxide (BPO) were added. Heat to 45°C, adjust to a suitable stirring speed and stir for 30 minutes, raise the temperature to 75°C for 3 hours, raise the temperature to 85°C for 2 hours, and continue to raise the temperature to 95°C for 3 hours. After cooling, alternately wash the resin with absolute ethanol, hot water, and cold water until the washing solution is clear, put it into a Soxhlet extractor and extract it with petroleum ether for 12 hours, and dry it in vacuum for 24 ...

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Abstract

The invention discloses a method for preparing a polar modified ultrahighly-crosslinked resin and application of the resin. The method comprises the following steps: carrying out ternary suspension copolymerization on 4-vinylbenzyl chloride, acrylate and divinylbenzene to obtain a terpolymer precursor resin; carrying out Friedel-Crafts reaction on the obtained terpolymer precursor resin under the catalytic action of Lewis acid to obtain an ultrahighly-crosslinked resin; and after the ultrahighly-crosslinked resin is put in an amination reagent for swelling, carrying out amination reaction to obtain the polar modified ultrahighly-crosslinked resin with high specific area, large pore volume, proper pore size and proper polarity magnitude. The polar modified ultrahighly-crosslinked resin can be used for adsorbing polar small-molecule aromatic organic compounds in water, and has wide application prospects. Besides, the method for preparing the polar modified ultrahighly-crosslinked resin is simple, is low in cost, and can implement industrial production.

Description

technical field [0001] The invention relates to a method and application for preparing a polar-modified ultra-high cross-linked resin, belonging to the field of 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 ultra-high cross-linked resin. Ultra-highly cross-linked 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, storage and separation of gases, and other fields. [0003] However, the skeleton structure of ultra-highly cross-linked resins is hydrophobic polystyrene. On the one hand, its strong hydrophobicity mak...

Claims

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Application Information

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IPC IPC(8): C08F212/14C08F220/14C08F220/18C08F212/36C08F8/32C08J3/24B01J20/26B01J20/30B01D53/02
Inventor 黄健涵伏振宇王云秋刘又年李河冰闫冲陈立妙
Owner CENT SOUTH UNIV
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