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Super-crosslinked polymer, and preparation method and application thereof

A polymer and hypercrosslinking technology, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve problems such as environmental pollution, unfavorable industrial scale-up production, etc., and achieve the effect of mild reaction conditions and high adsorption capacity

Active Publication Date: 2020-02-21
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Description
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  • Application Information

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Problems solved by technology

[0004] The above-mentioned methods for preparing HCPs use low-boiling point solvents and reaction systems, and adopt methods such as segmental heating and reflux to realize polymerization reactions, which not only require heating in different stages, but also require a certain reaction time for each stage, which is not conducive to industrial scale-up production. Simultaneously, the Friedel-Crafts alkylation reaction catalyst that adopts all requires anhydrous such as ferric chloride, aluminum chloride, zinc chloride etc., produces a large amount of catalyst wastes after polymerization, can pollute the environment

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  • Super-crosslinked polymer, and preparation method and application thereof
  • Super-crosslinked polymer, and preparation method and application thereof
  • Super-crosslinked polymer, and preparation method and application thereof

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preparation example Construction

[0031] The invention provides a kind of preparation method of hypercrosslinked polymer, comprises the following steps:

[0032] Mix 2,3,5,6-tetrafluoroterephthalaldehyde, aromatic hydrocarbons, halogenated hydrocarbon solvents and catalysts for polymerization to obtain hypercrosslinked polymers;

[0033] Described catalyst is trifluoromethanesulfonic acid;

[0034] The temperature of the polymerization reaction is 20-35°C, and the time is 30min-2h.

[0035] In the present invention, unless otherwise specified, the required preparation materials are commercially available products well known to those skilled in the art.

[0036] The invention mixes 2,3,5,6-tetrafluoro terephthalaldehyde, aromatic hydrocarbon, halogenated hydrocarbon solvent and catalyst. In the present invention, the aromatic hydrocarbon is preferably benzene, biphenyl, 1,4-diphenylbenzene, 1,3,5-triphenylbenzene or tetraphenylmethane; the aromatic hydrocarbon and 2,3, The molar ratio of 5,6-tetrafluoroterep...

Embodiment 1

[0050] At 20°C, mix 0.206g (1.0mmol) of 2,3,5,6-tetrafluoroterephthalaldehyde and 0.148g (1.90mmol) of benzene in 0.206g of dichloromethane at a stirring speed of 120rpm. , drop trifluoromethanesulfonic acid 0.075g (0.5mmol, TFSA), then carry out polymerization reaction 30min, after the reaction is completed, the product obtained is poured into ethanol, and the product obtained is ground to obtain a powder, and the powder is deionized Soaking in water, washing, grinding, and vacuum drying yielded 0.325 g of a hypercrosslinked polymer, denoted as HCP-TF-1, with a yield of 92%.

[0051] The reaction process of the present embodiment is as follows:

[0052]

Embodiment 2

[0054] At 35°C, mix 0.206g (1.0mmol) of 2,3,5,6-tetrafluoroterephthalaldehyde with 0.301g (1.95mmol) of biphenyl in 0.618g of 1,2-dichloroethane, stirring at Be 200rpm, after stirring evenly, drip trifluoromethanesulfonic acid 0.113g (0.75mmol, TFSA), carry out polymerization reaction 30min then, after the reaction is finished, the gained product is poured into ethanol, and the gained product is obtained powder through grinding again, will The powder was soaked and washed in deionized water, ground, and vacuum-dried to obtain 0.486 g of a hypercrosslinked polymer, denoted as HCP-TF-2, with a yield of 96%.

[0055] The reaction process of the present embodiment is as follows:

[0056]

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Abstract

The invention belongs to the technical field of super-crosslinked polymers, and particularly relates to a super-crosslinked polymer, and a preparation method and application thereof. According to theinvention, a polymerization reaction system with mild reaction conditions is adopted; 2,3,5,6-tetrafluoroterephthalaldehyde and aromatic hydrocarbon are used as monomers, and halogenated hydrocarbon is used as a solvent; a super-crosslinking polymerization reaction can be quickly completed at room temperature in the presence of trifluoromethanesulfonic acid without heating so as to generate the super-crosslinked polymer; a high specific surface area can be obtained in a reaction period smaller than 2 hours, the defects of segmented heating, long-time reaction and the like in traditional methods for preparing the super-crosslinked polymer are overcome, and preparation efficiency is improved; and the prepared super-crosslinked polymer has a specific surface area (BET) of 815-1776 m<2> / g, a pore diameter of 2-20nm and a pore volume of 0.63-3.26 cm<3> / g, and the super-crosslinked polymer has potential application prospects in the field of gas adsorption and storage due to the high specificsurface area and pore volume.

Description

technical field [0001] The invention relates to the technical field of hypercrosslinked polymers, in particular to a hypercrosslinked polymer and its preparation method and application. Background technique [0002] Porous organic polymer materials have attracted more and more attention because of their high specific surface area, low density, good thermal and chemical stability, and excellent chemical designability. Heterogeneous catalysis, toxic gas sensing, and energy storage and conversion have broad application prospects. Hyper-Crosslinking Polymers (HCPs) is a class of organic porous materials prepared based on Friedel-Crafts alkylation reaction. It borrows and extends the concept of "crosslinking" used in the synthesis of other materials. During the preparation of HCPs, the degree of cross-linking is greater, and the obtained polymer network exhibits a high degree of rigidity, which strongly prevents the tight shrinkage of polymer chains, so that the gaps existing be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G10/02B01J20/26B01J20/30B01D53/02
CPCB01D53/02B01J20/267C08G10/02
Inventor 陶立明张耀明王廷梅王齐华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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