Preparation method and application of hypercrosslinked resin with controllable polarity and pore structure

A technology of ultra-high cross-linked resin and pore structure, which is applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., and can solve problems such as difficult control of pore size and complicated production steps

Inactive Publication Date: 2016-09-07
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 prov

Method used

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  • Preparation method and application of hypercrosslinked resin with controllable polarity and pore structure
  • Preparation method and application of hypercrosslinked resin with controllable polarity and pore structure
  • Preparation method and application of hypercrosslinked resin with controllable polarity and pore structure

Examples

Experimental program
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Example Embodiment

[0040] Example 1

[0041] 1) Preparation of precursor resin:

[0042] Place a 500mL three-necked round bottom flask on a water bath device equipped with a mechanical stirrer, condenser and thermometer. First add the water phase (180mL of distilled water, 20mL of 1% polyvinyl alcohol, and 5 drops of methylene blue). Add 40 g of oil adjacent xylene and benzyl alcohol, 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, heat up to 75°C for 2h, heat up to 85°C for 3h, continue to heat up to 95°C for 3h. After cooling, the resin was washed alternately with absolute ethanol, hot water and cold water until the washing liquid was clarified, extracted with petroleum ether for 12 hours in a Soxhlet extractor, and dried in vacuum for 24 hours to obtain the precursor resin PEV-x-ab, (where , X is the mass percentage of crosslinking agent ethylene glyc...

Example Embodiment

[0047] Example 2

[0048] 1) Preparation of precursor resin:

[0049] Place a 500mL three-necked round bottom flask on a water bath device equipped with a mechanical stirrer, condenser and thermometer. First add the water phase (180mL of distilled water, 20mL of 1% polyvinyl alcohol, and 5 drops of methylene blue). Add 40g of oil adjacent xylene and benzyl alcohol, 20g of 1,4-butanediol dimethacrylate (BDDMA) and 4-vinylbenzyl chloride (VBC), and 0.2g of azobisisobutyronitrile (AIBN) . Heat to 45°C, adjust to a suitable stirring speed and stir for 30 minutes, warm to 75°C for 3 hours, warm to 85°C to react for 4 hours, and continue to warm to 95°C to react for 5 hours. After cooling, the resin was washed alternately with absolute ethanol, hot water and cold water until the washing liquid was clear, extracted with petroleum ether for 12 hours in a Soxhlet extractor, and dried under vacuum for 24 hours to obtain the precursor resin PBV-x-ab: x said The mass percentage of crosslink...

Example Embodiment

[0054] Example 3

[0055] 1) Preparation of precursor resin:

[0056] Place a 500mL three-necked round bottom flask on a water bath device equipped with a mechanical stirrer, condenser and thermometer. First add the water phase (180mL of distilled water, 20mL of 1% polyvinyl alcohol, and 5 drops of methylene blue). Add 40 g of oil adjacent xylene and benzyl alcohol, 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, warm up to 75°C for 5 hours, warm up to 85°C for 3 hours, and continue to warm to 95°C for 3 hours. After cooling, the resin was washed alternately with absolute ethanol, hot water and cold water until the washing liquid was clarified, extracted with petroleum ether for 12 hours in a Soxhlet extractor, and dried in vacuum for 24 hours to obtain the precursor resin PPV-x-ab.

[0057] 2) Friedel-Crafts reaction:

[0058] Add 15 g of ...

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Abstract

The invention discloses a preparation method and application of hypercrosslinked resin with controllable polarity and pore structure. The preparation method of the hypercrosslinked resin comprises the following steps: taking dimethyl acrylate as a crosslinking agent, taking 4-vinyl benzyl chloride as a monomer, carrying out suspension polymerization in the presence of a pore-foaming agent, a dispersant and an initiator to obtain precursor resin; and carrying out Friedel-Crafts reaction on the precursor resin under the catalytic action of lewis acid to obtain the hypercrosslinked resin. By regulating the mass ratio of the crosslinking agent to the monomer, the polarity and the pore structure of the hypercrosslinked resin can be controlled within a certain range; meanwhile, the polarity and the pore structure of the hypercrosslinked resin can be regulated within a proper range; the hypercrosslinked resin can be used for selectively adsorbing polar micromolecule aromatic organic compounds and has a wide application prospect; in addition, the preparation method of the hypercrosslinked resin is simple and is low in cost; the prepared hypercrosslinked resin is excellent in dynamic properties and high in reusability, and is suitable for industrial production.

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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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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