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Method for preparing super-macroporous high-specific-area polymer

A high specific surface area, polymer technology, applied in the field of polymer materials, can solve problems such as small adsorption capacity, and achieve the effects of simple post-processing, simple and reliable preparation method, and high specific surface area

Inactive Publication Date: 2017-02-15
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN100562530C discloses a preparation method of super-macroporous polymer microspheres, using styrene and the like as monomers, divinylbenzene as crosslinking agents, and cyclohexanol as porogens to prepare super-macroporous microspheres by suspension polymerization , the pore size distribution of the obtained microspheres is between 10-200 nm and 1-60 μm, and the highest specific surface area can only reach 203.8 m 2 / g, so the adsorption capacity of such materials is usually small

Method used

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  • Method for preparing super-macroporous high-specific-area polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Dissolve 4.0 ml of divinylbenzene monomer in 16 ml of dimethyl sulfoxide, add 36.8 mg of benzoyl peroxide, 19 μl of N,N-dimethylaniline, mix well, blow nitrogen for 5 min to remove oxygen, and After reacting at 18°C ​​for 96 hours, place it at room temperature until the crystals of dimethyl sulfoxide melt, wash thoroughly with methanol, then wash with deionized water to remove methanol, put it in an oven at 50°C and bake to constant weight to obtain super-macroporous polymer thing. The obtained polymer has a specific surface area of ​​140.35 m 2 / g.

Embodiment 2

[0031] Take 20 ml dichloroethane and 40 mg anhydrous FeCl 3In the reaction kettle, ultrasonically disperse, add 100 mg of the polymer precursor obtained in Example 1, pass through nitrogen for 10 minutes, remove oxygen, seal, swell for 1 hour, then place it in an oil bath at 85 ° C for 18 hours, cool Afterwards, it was fully washed with methanol, washed with 0.1 mol / L hydrochloric acid, soaked, rinsed with deionized water, and dried in an oven at 50 °C to constant weight to obtain a polymer with super large pores and high specific surface area. The specific surface area of ​​the obtained polymer is 1214.19m 2 / g.

Embodiment 3

[0033] Take 20 ml of dichloroethane and 10 mg of benzoyl peroxide in a reaction kettle, dissolve them, add 100 mg of the polymer precursor obtained in Example 1, blow in nitrogen for 10 minutes, remove oxygen, seal and swell for 1 hour , and then placed in an oil bath at 85 °C for 18 hours, cooled, washed thoroughly with methanol, and then washed with deionized water, and dried in an oven at 50 °C to constant weight to obtain a polymer with super large pores and high specific surface area. The specific surface area of ​​the obtained polymer is 84.77 m 2 / g.

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Abstract

The invention relates to a method for preparing a super-macroporous high-specific-area polymer. The method includes obtaining a super-macroporous polymer through low-temperature freezing polymerization, and subjecting the super-macroporous polymer to post-crosslinking through free radical reaction or Friedel-Crafts alkylation reaction so as to obtain the super-macroporous high-specific-area polymer. The method further includes taking a divinyl benzene as a monomer, dimethyl sulfoxide as a solvent and a crystal as a pore-foaming agent, selecting a redox initiation system and polymerizing to obtain the super-macroporous polymer; taking the super-macroporous polymer as a precursor and dichloroethane as a solvent, adding a free radical initiator or ferric trichloride to perform post-crosslinking, carrying out thermostatic reaction in oil bath at 85 DEG C for 18 hours, washing and drying so as to obtain the super-macroporous high-specific-area polymer. The method is simple and reliable and simple in post-treatment. The super-macroporous high-specific-area polymer has a super-macroporous structure and a high specific area, the pore size range is mainly between 5-100 nm and 20-200 micrometers, and the maximum specific area can be up to 1214.19 m<2> / g.

Description

technical field [0001] The invention relates to a method for preparing a polymer with super large pores and high specific surface area, belonging to the technical field of polymer materials. Background technique [0002] Porous materials have a wide range of applications in many fields such as adsorption, catalysis, surface reaction, and gas storage due to their high specific surface area. [0003] At present, post-crosslinking reaction is one of the main methods to prepare polymeric porous materials with high specific surface area. The post-crosslinking reaction refers to the construction of new connection points in the initial polymer network structure, thereby generating more crosslinking sites on the polymer skeleton structure and fixing them, making the intertwined polymer molecular segments more Stable chemical reaction process. It can be divided into Friedel-Crafts post-crosslinking (Jou-Hyeon Ahn, Jin-Eon Jang, Chang-Gun Oh, Son-Ki Ihm, JamieCortez, David C. Sherri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/36C08F212/12C08F4/40C08J9/28C08J3/24
CPCC08F4/40C08F212/36C08J3/24C08J9/286C08J2201/026C08J2201/0502C08J2325/02C08F212/12
Inventor 王银萍陈喜禄陈志勇
Owner UNIV OF JINAN
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