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Segmented copolymer of side chain sulfonated type polyimide and sulfonated polybutadiene and preparation method thereof

A technology of sulfonated polybutadiene and block copolymers, which is applied in the direction of electrochemical generators, structural parts, battery pack parts, etc., and can solve problems such as easy loss and high price of perfluorosulfonic acid proton exchange membranes , to simplify the synthesis, ensure the reaction conversion rate and improve the hydrolysis stability

Active Publication Date: 2010-05-05
南雄市毅豪化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this perfluorosulfonic acid-type proton exchange membrane is expensive, and it is easy to lose many excellent properties at high temperatures
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Method used

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  • Segmented copolymer of side chain sulfonated type polyimide and sulfonated polybutadiene and preparation method thereof
  • Segmented copolymer of side chain sulfonated type polyimide and sulfonated polybutadiene and preparation method thereof
  • Segmented copolymer of side chain sulfonated type polyimide and sulfonated polybutadiene and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (a) Dissolve 3.25g of carboxy-terminated polybutadiene in 30g of toluene, add 3g of thionyl chloride and stir evenly; rise to 60°C for 3 hours under nitrogen protection, then rise to 110°C for 12 hours After the reaction is finished, cool down, and remove the remaining thionyl chloride by distillation under reduced pressure, so as to obtain the toluene solution of terminal acid chloride polybutadiene:

[0034] (b) Add 11.525g of 3,5-dinitrobenzoyl chloride and 8.5g of anhydrous aluminum trichloride to a three-neck round bottom flask, and stir slowly under ice bath conditions; slowly add 8.5g of diphenyl diphenyl chloride dropwise within 1 hour After ether, react for 30 minutes; then heat to 50°C under the protection of nitrogen, and continue to react for 12 hours; cool the reaction solution, pour it into ice hydrochloric acid solution to precipitate, stir, filter, wash the crude product, and vacuum dry to obtain 3 , 5-dinitro-4'-phenoxybenzophenone;

[0035](c) Add 3.6...

Embodiment 2

[0044] (a) Dissolve 6.5g of carboxy-terminated polybutadiene in 40g of toluene, add 6g of thionyl chloride and stir evenly; rise to 70°C for 2 hours under nitrogen protection, then rise to 100°C for 15 hours After the reaction is finished, cool down, and remove the remaining thionyl chloride by distillation under reduced pressure, so as to obtain the toluene solution of polybutadiene with acyl chloride terminal;

[0045] (b) Add 23.05g 3,5-dinitrobenzoyl chloride and 17g anhydrous aluminum trichloride to the three-neck round bottom flask, and stir slowly under ice bath conditions; after slowly adding 17g diphenyl ether in 1.5 hours , reacted for 60 minutes; then heated to 60°C under the protection of nitrogen, and continued to react for 18 hours; cooled the reaction solution, poured it into ice hydrochloric acid solution to precipitate, stirred, filtered, washed the crude product, and vacuum dried to obtain 3,5 - dinitro-4'-phenoxybenzophenone;

[0046] (c) Add 7.28g 3,5-dini...

Embodiment 3

[0055] (a) Dissolve 9.75g of carboxyl-terminated polybutadiene in 50g of toluene, add 9g of thionyl chloride and stir evenly; rise to 80°C for 1 hour under nitrogen protection, then rise to 90°C for 18 hours After the reaction is finished, cool down, and remove the remaining thionyl chloride by distillation under reduced pressure, so as to obtain the toluene solution of polybutadiene with acyl chloride terminal;

[0056] (b) Add 34.575g 3,5-dinitrobenzoyl chloride and 25.5g anhydrous aluminum trichloride to the three-neck round bottom flask, and stir slowly under ice bath conditions; slowly add 25.5g diphenyl diphenyl chloride dropwise in 2 hours After ether, react for 90 minutes; then heat to 70°C under the protection of nitrogen, and continue to react for 24 hours; cool the reaction solution, pour it into ice hydrochloric acid solution for precipitation, stir, filter, wash the crude product with water, and vacuum dry to obtain 3 , 5-dinitro-4'-phenoxybenzophenone;

[0057] ...

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Abstract

The invention relates to a segmented copolymer of side chain sulfonated type polyimide and sulfonated polybutadiene and a preparation method thereof. The preparation method comprises the following steps: firstly synthesizing a novel sulfonated diammine monomer, polymerizing the monomer and naphthalenetetracarboxylic dianhydride which are used as raw materials to obtain terminal amino side chain sulfonated type polyimide; modifying terminal carboxyl polybutadiene by using thionyl chloride to obtain terminal acyl chloro polybutadiene; carrying out polycondensation reaction on the two preformed polymers under an waterless condition, and synthesizing to obtain the segmented copolymer of the side chain sulfonated type polyimide and the polybutadiene; and finally selectively sulfonating the segmented copolymer by using acetyl sulface prepared from concentrated sulfuric acid and acetic anhydride to obtain the segmented copolymer of the side chain sulfonated type polyimide and the sulfonated polybutadiene. The segmented copolymer is dissolved in an organic solvent and is coated with a film to prepare a proton exchange film for a fuel cell. The film has good proton electric conductivity and hydrolytic stability, and has extensive application prospects in the field of proton exchange films for fuel cells.

Description

technical field [0001] The invention relates to a side chain sulfonated polyimide and sulfonated polybutadiene block copolymer and a preparation method thereof. The prepared copolymer can be applied to the preparation of fuel cell proton exchange membranes and belongs to functional polymers field of materials technology. Background technique [0002] Fuel cell is an important energy conversion device. Due to its high efficiency, low noise, and low pollution, it has broad application prospects in the fields of automobile power, stationary electric energy, and portable power. Proton exchange membranes are key components in fuel cells. The representative of the highest level of proton exchange membranes today is the Nafion membrane produced by DuPont in the late 1960s. It has a crystallizable hydrophobic tetrafluoroethylene main chain and multiple perfluoroethylene terminated by perfluorosulfonic acid groups. Ether side chains [Alternative Polymer Systems for Proton Exchange ...

Claims

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Application Information

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IPC IPC(8): C08G81/02C08G73/10C08F8/18C08F136/06C08J5/22H01M2/16H01M8/02H01M8/0202H01M8/1016H01M8/1069H01M50/411H01M50/497
CPCY02E60/12Y02E60/50
Inventor 印杰赵渊
Owner 南雄市毅豪化工有限公司
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