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Preparation method of crown ether-containing copolymerized polyimide and phosphoric acid-doped proton exchange membrane prepared from same

A technology of proton exchange membrane and polyimide, which is applied in electrochemical generators, fuel cells, electrical components, etc., can solve the problems of low conductivity and low service temperature of proton exchange membranes, and achieve good mechanical properties and good durability The effect of thermal stability

Active Publication Date: 2021-08-31
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conductivity of the proton exchange membrane prepared by the above-mentioned sulfonated polyimide is low, the operating temperature is low and high humidity is required, and the preparation of the high-temperature polyimide proton exchange membrane needs to introduce substituents such as benzimidazole, which is complicated, so it is urgent to prepare A phosphoric acid-doped crown ether-containing copolymerized polyimide proton exchange membrane with low humidity and high conductivity from low temperature to high temperature

Method used

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  • Preparation method of crown ether-containing copolymerized polyimide and phosphoric acid-doped proton exchange membrane prepared from same
  • Preparation method of crown ether-containing copolymerized polyimide and phosphoric acid-doped proton exchange membrane prepared from same
  • Preparation method of crown ether-containing copolymerized polyimide and phosphoric acid-doped proton exchange membrane prepared from same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] This embodiment provides a kind of crown ether-containing copolymerized polyimide, its structural formula is as follows:

[0060]

[0061] The specific preparation method is as follows:

[0062] (1) Preparation of diamine monomer A containing imide chain segments

[0063] Add the aliphatic diamine BACH (15.9834g, 60mmol) into a 500mL three-neck flask under nitrogen protection, then add 150mL of NMP, after the aliphatic diamine is completely dissolved, then add the aromatic dianhydride PTCDA (7.8464g, 20mmol) , stirred and reacted at 80°C for 12 hours, after the reaction was completed, cooled to room temperature, added 50 mL of water-carrying agent toluene, and stirred and refluxed at 180°C for 9 hours to obtain a solution of diamine monomer A containing imide chains, After the toluene is completely distilled off, stop heating, and after naturally cooling to normal temperature, pour the reaction solution into a mixture of methanol and water (2L, V 甲醇 :V 水 = 1:1), a...

Embodiment 2

[0071] This embodiment provides a kind of crown ether-containing copolymerized polyimide, its structural formula is as follows:

[0072]

[0073] The specific preparation method is as follows:

[0074] (1) Preparation of diamine monomer A containing imide chain segments

[0075] Add the aromatic diamine o-Tolidine (12.738g, 60mmol) into a 500mL three-necked flask under nitrogen protection, and then add 150mL of NMP. After the o-Tolidine is completely dissolved, add the aromatic dianhydride BPDA (5.8844g, 20mmol ), stirred and reacted at 0°C for 24 hours, after the reaction was completed, 50 mL of water-carrying agent toluene was added, stirred and refluxed at 200°C for 8 hours, and a solution of diamine monomer A containing imide chain segments was obtained. After the o-xylene was released, stop heating, and after naturally cooling to normal temperature, the reaction solution was poured into a mixture of ethanol and water (2L, V 甲醇 :V 水 = 1:1), a precipitate was precipit...

Embodiment 3

[0083] This example provides a crown ether-containing copolymerized polyimide and its phosphoric acid-doped proton exchange membrane. The difference between the preparation method and Example 1 is that the diamine monomer A in step (2) is 1.6 g, and the crown ether Diamine monomer R 3 Be 0.060g, the ratio of the amount of both substances is 9:1, and other steps are identical with embodiment 1.

[0084] Structure Characterization:

[0085] Fourier transform infrared spectroscopy (FTIR) showed that the polymer was at 1371cm -1 , 1715cm -1 , 1781cm -1 The absorption peak of the imide ring is shown nearby;

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Abstract

The invention provides a preparation method of crown ether-containing copolymerized polyimide and a phosphoric acid-doped proton exchange membrane prepared from the same. The crown ether-containing copolymerized polyimide has a structure as shown in a formula I, can be used as a phosphoric acid doped proton exchange membrane material, and is obtained by synthesizing a diamine monomer A containing an imide chain link and a diamine monomer B containing a crown ether ring by adopting dianhydride and diamine and polymerizing the diamine monomers under the action of an origin agent. A molecular chain of the copolymerized polyimide provided by the invention has a Troger's base structure, and a main chain contains a crown ether structure. The prepared copolymerized polyimide has excellent film-forming property and mechanical property and relatively high thermal stability. The phosphoric acid doped proton exchange membrane is good in mechanical property, high in hydrolysis resistance and oxidation resistance and good in dimensional stability, has good conductivity in low-temperature to high-temperature and low-humidity environments, and has a wide application prospect as a fuel cell wide-temperature-range proton exchange membrane.

Description

[0001] The invention belongs to the technical field of new polyimide materials, and in particular relates to a method for preparing a crown ether-containing copolymerized polyimide and a phosphoric acid-doped proton exchange membrane. Background technique [0002] In order to find an alternative energy source to fossil fuels, fuel cells, which directly convert the chemical energy of fuels such as hydrogen and methanol into electrical energy, have been extensively studied. Among various types of fuel cells, proton exchange membrane fuel cells (PEMFCs) are particularly important because they can be used as portable, vehicular, and stationary energy sources. Traditional perfluorosulfonic acid proton exchange membranes represented by Nafion, Flemion, Aciplex and Dow have excellent electrical conductivity and chemical corrosion resistance, and are widely used in proton exchange membranes and industries. Currently, the most studied high-temperature proton exchange membranes are phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L79/08C08J5/22H01M8/1088H01M8/1081H01M8/103
CPCC08G73/1071C08G73/1007C08J5/2256C08J5/2287H01M8/1088H01M8/1081H01M8/103C08J2379/08Y02E60/50
Inventor 庄永兵张宇陆英杰朱浩万印华
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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