Aqueous polyimide precursor solution composition and method for producing aqueous polyimide precursor solution composition
a technology of aqueous polyimide and solution composition, which is applied in the direction of electrochemical generators, cell components, electrolytic capacitors, etc., can solve the problems of limited application, high cost, and inability to meet the requirements of aqueous polyimide solution composition, etc., and achieves easy production, high environmental acceptability, and easy production
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[0197]Hereinafter, the present invention will be more specifically described with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples.
[0198]The methods for measuring the properties, which was used in the following examples, will be described below.
[0199]A sample solution (the weight is referred to as “w1”) was heated at 120° C. for 10 minutes, 250° C. for 10 minutes, and then 350° C. for 30 minutes in a hot air dryer, and the weight of the sample after the heat treatment (the weight is referred to as “w2”) was measured. The solid content [wt %] was calculated by the following formula.
Solid content [wt %]=(w2 / w1)×100
[0200]A sample solution was diluted to a concentration of 0.5 g / dl based on the solid content (the solvent: water). The flowing time (T1) of the diluted solution was measured at 30° C. using a Cannon-Fenske viscometer No. 100. The inherent viscosity was calculated by the following formula using the flowing time (T0) o...
example a1
[0231]In a 500 mL (internal volume) glass reaction vessel equipped with a stirrer and a nitrogen-gas charging / discharge tube was placed 450 g of water as a solvent. And then, 13.44 g (0.124 mol) of PPD and 29.87 g (1.25 equivalents per carboxyl group) of 1,2-DMZ were added thereto, and the mixture was stirred at 25° C. for 1 hour to dissolve these compounds in water. Subsequently, 36.56 g (0.124 mol) of s-BPDA was added to the resulting solution, and the mixture was stirred at 25° C. for 12 hours to provide an aqueous polyimide precursor solution having a solid content of 9.0 wt %, a solution viscosity of 16.3 Pa·s, and an inherent viscosity of 0.95.
[0232]The properties of the aqueous polyimide precursor solution composition and the polyimide film obtained are shown in Table 1.
example a2
[0233]In a 500 mL (internal volume) glass reaction vessel equipped with a stirrer and a nitrogen-gas charging / discharge tube was placed 450 g of water as a solvent. And then, 13.44 g (0.124 mol) of PPD and 29.87 g (1.25 equivalents per carboxyl group) of 1,2-DMZ were added thereto, and the mixture was stirred at 25° C. for 1 hour to dissolve these compounds in water. Subsequently, 36.56 g (0.124 mol) of s-BPDA was added to the resulting solution, and the mixture was stirred at 50° C. for 8 hours to provide an aqueous polyimide precursor solution having a solid content of 9.1 wt %, a solution viscosity of 35.5 Pa·s, and an inherent viscosity of 1.25.
[0234]The properties of the aqueous polyimide precursor solution composition and the polyimide film obtained are shown in Table 1.
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