Preparation method and application of a kind of ultra-high cross-linked resin with controllable polarity and pore structure

A technology of ultra-high cross-linking resin and pore structure, which is applied in the preparation of ultra-high cross-linking resin, the application of ultra-high cross-linking resin in the adsorption of polar aromatic organic compounds, and the field of controllable preparation of ultra-high cross-linking resin , which can solve the problems of complex production steps and difficult adjustment of pore size

Inactive Publication Date: 2018-06-05
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the defects of super-high cross-linked resins in the prior art, such as hydrophobicity, difficult regulation of pore size, and complicated production steps, the purpose of the present invention is to provide a method for preparing super-high cross-linked resins that can realize arbitrary regulation of pore structure and polarity. method, the method is simple to operate, low in cost, and satisfies industrialized production

Method used

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  • Preparation method and application of a kind of ultra-high cross-linked resin with controllable polarity and pore structure
  • Preparation method and application of a kind of ultra-high cross-linked resin with controllable polarity and pore structure
  • Preparation method and application of a kind of ultra-high cross-linked resin with controllable polarity and pore structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1) Preparation of precursor resin:

[0042] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. Add a total of 40 g of oil-o-xylene and benzyl alcohol, a total of 20 g of ethylene glycol dimethacrylate (EGDMA) and 4-vinylbenzyl chloride (VBC), and 0.2 g of azobisisobutyronitrile (AIBN). Heat to 45°C, adjust to a suitable stirring speed and stir for 30min, raise the temperature to 75°C for 2h, raise the temperature to 85°C for 3h, continue to raise the temperature to 95°C for 3h. 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 for 12 h in a Soxhlet extractor, and dried in vacuum for 24 h to obtain the precursor resin PEV-x-ab, (where , x is the mass percent of the crosslinking agent ethylene glycol dimethacrylate; a:b is the relative mass ratio of o-xylene and benzyl alcohol ...

Embodiment 2

[0048] 1) Preparation of precursor resin:

[0049] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. Add a total of 40g of oil ophthalmic xylene and benzyl alcohol, a total of 20g of 1,4-butanediol dimethacrylate (BDDMA) and 4-vinylbenzyl chloride (VBC), 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 75°C for 3 hours, raise the temperature to 85°C for 4 hours, and continue to raise the temperature to 95°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 PBV-x-ab: represented by x The crosslinking agent is 1,4 butanediol dimethacrylate by mass percentage, a:b is the relative ma...

Embodiment 3

[0055] 1) Preparation of precursor resin:

[0056] Place a 500mL three-necked round-bottomed flask on a water bath equipped with a mechanical stirrer, a condenser, and a thermometer. Add a total of 40 g of oil ophthalmic xylene and benzyl alcohol, a total of 20 g of glycerol dimethacrylate (PGDMA) and 4-vinylbenzyl chloride (VBC), and 0.2 g of azobisisobutyronitrile (AIBN). Heat to 45°C, adjust to a suitable stirring speed and stir for 30 minutes, raise the temperature to 75°C for 5 hours, raise the temperature to 85°C for 3 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 liquid was clear, extracted with petroleum ether in a Soxhlet extractor for 12 hours, and dried in vacuum for 24 hours to obtain the precursor resin PPV-x-ab.

[0057] 2) Friedel-Crafts reaction:

[0058] Add 15g of precursor resin PPV-10%-ab and 90mL of 1,2-dichloroethane int...

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Abstract

The invention discloses a preparation method and application of an ultra-high cross-linked resin with controllable polarity and pore structure. The preparation method of the ultra-high cross-linked resin is to use dimethacrylate as the cross-linking agent, 4-vinylbenzyl chloride as the monomer, and obtain the precursor resin by suspension polymerization in the presence of porogens, dispersants and initiators ; The resulting precursor resin is subjected to a Friedel-Crafts reaction under Lewis acid catalysis to obtain an ultra-highly cross-linked resin. By adjusting the mass ratio of cross-linking agent to monomer, the polarity and pore structure of the ultra-high cross-linked resin can be adjusted within a certain range, and the polarity and pore structure of the ultra-high cross-linked resin can be adjusted in an appropriate range It can be used to selectively adsorb polar small molecular aromatic organic compounds in water, and has broad application prospects. In addition, the method for preparing the ultra-high cross-linked resin is simple, low in cost, excellent in dynamic performance, good in reusability, and can be industrialized.

Description

technical field [0001] The present invention relates to a preparation method of ultra-high cross-linked resin, in particular to a controllable preparation method of ultra-high cross-linked resin, and the application of ultra-high cross-linked resin in the adsorption of polar aromatic organic compounds, which belongs to macromolecule synthetic field. 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 gase...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F212/14C08F222/14C08F222/20C08F2/18C08J9/28C08J3/24B01J20/26B01J20/28B01J20/30C02F1/28C02F101/30C02F101/34
CPCC02F1/285C08F2/18C08F212/14C08F222/1006C08J3/24C08J9/28B01J20/267B01J20/28061B01J20/28073B01J20/28083C08J2325/18C08J2335/02C02F2101/34C02F2101/345C02F2101/30C08F222/102C08F222/103
Inventor 黄健涵邵礼书霍嘉琪张婷刘明强刘又年梁成易承志
Owner CENT SOUTH UNIV
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