Method for manufacturing sulfonated polyimide membrane having alicyclic structure

Abstract

A method for manufacturing a sulfonated polyimide film with a dicyclopentadiene structure includes: a first step of dissolving benzidine disulfonic acid triethylamine salt and 3,3',4,4'-benzophenone tetracarboxylic dianhydride in dimethyl sulfoxide and reacting to obtain a first compound; a second step of dissolving 4,4'-oxodiphenylamine, tricyclodecanediethanol diacrylate and 3,3',4,4'-benzophenone tetracarboxylic dianhydride in dimethyl sulfoxide and reacting to obtain a second compound; a third step of mixing the first compound and the second compound and reacting to form a block copolymer solution; a fourth step of coating the block copolymer solution onto a substrate using a coating applicator; and a fifth step of heat-treating and cooling the coated substrate, and then peeling the formed sulfonated polyimide film with a dicyclopentadiene structure off the substrate.

Claims

1. A method for manufacturing a sulfonated polyimide film with a dicyclopentadiene structure, comprising: a first step of dissolving benzidine disulfonic acid triethylamine salt and 3,3',4,4'-benzophenone tetracarboxylic dianhydride in dimethyl sulfoxide, and reacting to obtain a polyimide fragment with an anhydride-terminated group as a first compound; a second step of dissolving 4,4'-oxodiphenylamine, tricyclodecanediethanol diacrylate and 3,3',4,4'-benzophenone tetracarboxylic dianhydride in dimethyl sulfoxide, and reacting to obtain a polyimide fragment with an amino-terminated group as a second compound; and a third step of mixing the first compound and the second compound, and reacting to form a block copolymer solution. The fourth step involves coating the block copolymer solution onto the substrate using a coating applicator; and the fifth step involves heat-treating and cooling the coated substrate, and then peeling off the resulting sulfonated polyimide film with a dicyclopentadiene structure from the substrate.

2. The manufacturing method as claimed in claim 1, wherein in the first step, the amount of benzidine disulfonic acid triethylamine salt is 1 to 10 mmol, the amount of 3,3',4,4'-benzophenone tetracarboxylic dianhydride is 1 to 10 mmol, the amount of dimethyl sulfoxide is 10 mL, and the solid content of the first compound is 15 to 20 wt%.

3. The manufacturing method as claimed in claim 1, wherein in the second step, the total amount of 4,4'-oxodiphenylamine and tricyclodecanediethanol diacrylate is 1 to 10 mmol, the mole number of tricyclodecanediethanol diacrylate is 5 to 10 mol% of the mole number of 4,4'-oxodiphenylamine, the amount of 3,3',4,4'-benzophenone tetracarboxylic dianhydride is 1 to 10 mmol, and the amount of dimethyl sulfoxide is 10 mL.

4. The manufacturing method as claimed in claim 1, wherein in the fifth step, heat treatment is performed sequentially by heating at 30 °C to 50 °C for 6 to 8 hours, heating at 80 °C to 150 °C for 1 to 3 hours, heating at 160 °C to 250 °C for 2 to 4 hours, and heating at 260 °C to 280 °C for 2 to 4 hours.

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