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Method for preparation of organic porous material based on cationic polymerization reaction

A porous material and organic technology, applied in the field of rapid preparation of organic porous materials based on cationic polymerization, can solve the problems of harsh reaction conditions and long reaction time, and achieve the effects of short reaction time, low cost and mild reaction conditions

Active Publication Date: 2019-07-05
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Previous studies have reported examples of organic porous polymers obtained by free radical polymerization of vinyl monomers using AIBN as an initiator under solvothermal conditions. However, the free radical polymerization method requires solvothermal conditions and an inert atmosphere. , the reaction time is longer, and the reaction conditions are still too harsh

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  • Method for preparation of organic porous material based on cationic polymerization reaction
  • Method for preparation of organic porous material based on cationic polymerization reaction
  • Method for preparation of organic porous material based on cationic polymerization reaction

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preparation example Construction

[0047]The solvent used in the preparation method of the organic porous polymer of the present invention is a halogenated solvent, preferably one or more of methyl chloride, methylene chloride, ethylene dichloride, chloroform or carbon tetrachloride.

[0048] The applicant of the present invention found in experiments that Lewis acid or protonic acid can be used as a catalyst to catalyze monomer polymerization, wherein anhydrous aluminum trichloride, anhydrous ferric chloride, anhydrous tin tetrachloride, anhydrous chlorinated Both zinc and concentrated sulfuric acid can catalyze the reaction polymerization. Among them, anhydrous ferric chloride and anhydrous aluminum trichloride have the highest catalytic activity and the fastest reaction rate, while the catalytic activity of zinc chloride is low, and dilute sulfuric acid cannot catalyze the reaction because the water content in dilute sulfuric acid is too high , water will quench the cationic active center.

[0049] The dosa...

Embodiment 1

[0057] Take 0.122g of 1,3,6,8-tetrakis(4-vinylphenyl)pyrene (TVP), add 15ml of 1,2-dichloroethane (DCE), and ultrasonically disperse evenly to obtain a green solution, stir, add 0.053g AlCl 3 , the color gradually became darker, dark green, and finally black, with bluish light on the edge of the liquid surface. After 36 hours of reaction, a large amount of ethanol was added to quench the reaction, and a large amount of light green precipitates were precipitated in the solution. Suction filter, wash with a large amount of ethanol several times, extract with ethanol for 24 hours, and dry in an oven at 60°C for 24 hours. A yellow solid was obtained in greater than 99% yield.

[0058] figure 2 It is a schematic diagram of the preparation reaction of this embodiment, and 1,3,6,8-tetrakis (4-vinylphenyl) pyrene has undergone a cross-linking polymerization reaction; image 3 , Figure 4 , Figure 5 with Image 6 Be respectively the infrared spectrum of embodiment 1 product, 1...

Embodiment 2

[0060] Take 0.122g of 1,3,6,8-tetrakis(4-vinylphenyl)pyrene (TVP), add 15ml of 1,2-dichloroethane (DCE), and ultrasonically disperse evenly to obtain a green solution, stir, add 0.065g FeCl 3 , the color gradually became darker, dark green, and finally black, with bluish light on the edge of the liquid surface. After 36 hours of reaction, a large amount of methanol was added to quench the reaction, and a large amount of light green precipitate was precipitated in the solution. Suction filter, wash with a large amount of methanol several times until the filtrate becomes colorless, extract with methanol for 24 hours, and dry in an oven at 60°C for 24 hours. A yellow-green solid was obtained in greater than 99% yield.

[0061] Figure 7 , Figure 8 , Figure 9 Be respectively the infrared spectrum of embodiment 2 product, nitrogen adsorption-desorption curve and pore size distribution curve, the BET of embodiment 2 product is 1549m 2 g -1 ,from Figure 8 with Figure 9 An...

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Abstract

Belonging to the technical field of new materials, the invention more specifically relates to a method for rapid preparation of an organic porous material based on cationic polymerization. The methodincludes: taking a binary or multi-element styryl aromatic ring compound dispersed in an organic solvent as the raw material, carrying out cationic polymerization reaction under the catalysis of a catalyst, and then performing separation and purification to obtain an organic porous polymer. The invention fully combines the characteristics and preparation requirements of organic porous materials, redesigns the preparation method specifically for organic porous materials, and selects and optimizes key preparation process raw materials and technological parameters, thus obtaining the organic porous material preparation method with the characteristics of mild conditions, fast reaction speed, convenient operation and high production efficiency accordingly.

Description

technical field [0001] The invention belongs to the technical field of new materials, and more specifically relates to a method for rapidly preparing organic porous materials based on cationic polymerization. Background technique [0002] Organic porous polymers (POPs) are composed of organic units through covalent bonds. They have the advantages of hierarchical pore structure, low skeletal density, and abundant monomer sources. They are used in gas adsorption storage, heterogeneous catalysis, sensing, Optoelectronics, energy storage and other aspects have shown broad application prospects, so they have attracted extensive attention from many research teams. [0003] The current synthesis methods of POPs mainly include: Suzuki-Miyaura reaction, Sonogashira reaction, Yamamoto reaction, free radical polymerization, Schiff-base reaction and Friedel-Crafts reaction, etc. However, most of these reactions use noble metal catalysts and high reaction temperatures, and the reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/34C08F112/36C08F4/14C08F4/26C08F4/16C08F4/10C08F4/30B01D53/02
CPCB01D53/02C08F112/34C08F112/36C08F4/14C08F4/26C08F4/16C08F4/10C08F4/30
Inventor 金尚彬程光谭必恩
Owner HUAZHONG UNIV OF SCI & TECH
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