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Method for preparing macromolecular adsorbents with large specific surface area

A high specific surface area, adsorbent technology, applied in the field of material chemistry, can solve the problems of high specific surface area polymer adsorbent production and use difficulties, etc., to achieve simple process, improved compression resistance and thermal stability, and increased crosslinking degree Effect

Active Publication Date: 2018-04-24
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method avoids the use of chloromethyl methyl ether, and some enterprises have adopted this process to produce high specific surface area polymer adsorbents, but this process still requires the use of dichloroethane, nitromethane, nitrobenzene and other highly volatile , Highly toxic solvents as swelling agents
[0005] In summary, the current mainstream polymer adsorbent crosslinking technology generally uses highly volatile and highly toxic reagents such as chloromethyl methyl ether and dichloroethane, which has brought great impact on the production and use of high specific surface area polymer adsorbents. It must be difficult, so it is inevitable to develop a green and environmentally friendly preparation process for the preparation of high specific surface area polymer adsorbents

Method used

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  • Method for preparing macromolecular adsorbents with large specific surface area

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] At room temperature, a premixed water phase was added to a 1L four-necked flask, and the composition was 484.5 g of deionized water, 15 g of sodium chloride, 0.5 g of polyvinyl alcohol, and 25 mg of methylene blue. Turn on the stirring and raise the temperature to 40°C. Turn off the stirring, add the oil phase premixed at normal temperature, and the composition is 66.7g of divinylbenzene, 16.7g of styrene, 41.7g of toluene, 41.7g of 3# white oil, and 0.8g of dibenzoyl peroxide. Turn on the stirring and adjust the speed according to the desired particle size. Raise the temperature to 80°C, keep the temperature constant for 6h, lower the system temperature to 50°C, add 66.7g of vinyl tris(β-methoxyethoxy)silane, 0.7g of di-tert-butylcyclohexyl peroxydicarbonate, and continue polymerization for 3h to obtain Copolymer beads.

[0037] After the copolymer beads were washed with water, the porogen in the beads was extracted with acetone as a solvent, and the mass ratio of ac...

Embodiment 2

[0044] At room temperature, a premixed water phase was added to a 1L four-neck flask, and the composition was 494.7g of deionized water, 5g of potassium chloride, 0.25g of gelatin, and 0.5mg of sodium nitrite. Turn on the stirring and raise the temperature to 60°C. Turn off the stirring, add the oil phase premixed at normal temperature, and the composition is 60g of trivinylbenzene, 15g of methylstyrene, 12.5g of xylene, 12.5g of 200# solvent naphtha, and 0.25g of azobisisobutyronitrile. Turn on the stirring and adjust the speed according to the desired particle size. Raise the temperature to 70°C, keep the temperature constant for 4 hours, lower the system temperature to 50°C, add 10 g of vinyltrimethoxysilane and 0.03 g of acetylperoxycyclohexanesulfonyl, continue polymerization for 2 hours, and obtain copolymer beads.

[0045] After the copolymer beads were washed with water, the porogen in the beads was extracted with methylal as a solvent, and the mass ratio of the methy...

Embodiment 3

[0048] At room temperature, a premixed water phase was added to a 1L four-neck flask, and the composition was 447.4 g of deionized water, 50 g of calcium chloride, 2.5 g of hydroxypropyl methylcellulose, and 50 mg of sodium thiosulfate. Turn on stirring, room temperature. Turn off the stirring, add the oil phase premixed at normal temperature, and the composition is 50 g of divinyltoluene, 12.5 g of ethyl styrene, 187.5 g of ethyl benzene, and 2.5 g of dibenzoyl peroxide. Turn on the stirring and adjust the speed according to the desired particle size. Raise the temperature to 95°C, keep the temperature constant for 10 hours, lower the system temperature to 65°C, add 150 g of vinyltriethoxysilane and 6 g of diisopropyl peroxydicarbonate, and continue polymerization for 4 hours to obtain copolymer beads.

[0049] After the copolymer beads were washed with water, methanol was used as a solvent to extract the porogen in the beads, and the mass ratio of methanol to copolymer bead...

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Abstract

The invention discloses a method for preparing macromolecular adsorbents with large specific surface area by means of step-by-step suspension copolymerization pelletization by the aid of sol-gel procedure of vinylsilane coupling agents. The method mainly includes steps of (1), carrying out step-by-step suspension copolymerization on the vinylsilane coupling agents, polyethylene aromatic monomers and ethylene aromatic monomers to obtain copolymer beads; (2), extracting pore-forming agents from the copolymer beads and then hydrolyzing and cross-linking the copolymer beads in acid environments toobtain the macromolecular adsorbents cross-linked after sol-gel treatment. The method has the advantages that the method includes simple procedures and is environmentally friendly, secondary cross-linking steps are carried out, and accordingly, reagents such as chloromethyl methyl ether and dichloroethane with high toxicity can be omitted; the compressive properties and the heat stability of themacromolecular adsorbents prepared by the aid of the method can be obviously improved.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a preparation method of a high specific surface area polymer adsorbent. Background technique [0002] Polymer adsorbent is a kind of highly cross-linked, three-dimensional network structure, porous and high specific surface area material, which is widely used in water treatment, natural product extraction, chemical purification, biopharmaceutical and other fields. [0003] The adsorption capacity of polymer adsorbents usually increases with the increase of specific surface area and pore volume. An effective way to increase specific surface area and pore volume is to increase the cross-linking degree of the adsorbent by increasing cross-linking chemical bonds. For example, the Chinese invention patent CN1046533A discloses a method for preparing a high specific surface area adsorbent. The polymer adsorbent with styrene as the main material is chloromethylated under the action of c...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F212/08C08F230/08C08F212/34C08F212/14C08F220/44C08F212/12C08F220/14C08F2/20C08J9/28B01J20/26B01J20/30B01J20/28
CPCB01J20/261B01J20/28047C08F212/14C08F212/34C08F212/36C08J9/28C08J2201/0502C08J2325/02C08F212/08C08F230/08C08F212/12C08F220/44C08F220/14C08F2/20
Inventor 欧洋潘波高俊民乔义涛孙家宽华卫琦
Owner WANHUA CHEM GRP CO LTD
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