A method for preparing ultra-large pore high specific surface area polymer

A high specific surface area, ultra-large pore technology, applied in the field of polymer materials, can solve the problem of small adsorption capacity, and achieve the effect of simple post-treatment, high specific surface area, and simple and reliable preparation method

Inactive Publication Date: 2018-11-27
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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  • A method for preparing ultra-large pore high specific surface area polymer

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Experimental program
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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 ℃ for 96 hours, place it at room temperature until the dimethyl sulfoxide crystals melt, wash fully with methanol, then wash with deionized water to remove methanol, put it in an oven at 50 ℃ and bake to constant weight to obtain a super-macroporous polymer . 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 1214.19 m 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 polymer with super large pores and high specific surface area. In the method, a super-macroporous polymer is firstly obtained by low-temperature freezing polymerization, and then post-crosslinked by free radical reaction or Friedel-Crafts alkylation reaction respectively to obtain a super-macroporous polymer with high specific surface area. Using divinylbenzene as a monomer, dimethyl sulfoxide as a solvent, and its crystal as a porogen, select a redox initiation system to polymerize to obtain a super-macroporous polymer, and then use this polymer as a precursor to dichloro Ethane is used as a solvent, post-crosslinking is carried out by adding a free radical initiator or ferric chloride, and a constant temperature reaction is carried out in an oil bath at 85° C. for 18 hours. After washing and drying, a polymer with super large pores and high specific surface area is obtained. The preparation method of the present invention is simple and reliable, and the post-treatment is simple. The obtained polymer not only has a super-macroporous structure, but also has a high specific surface area. Up to 1214.19 m2 / 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 Patents(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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