Polyimide with phosphoric acid side chain-containing long chain and preparation method and application thereof
A polyimide and phosphoric acid technology, which is applied in the parts of fuel cells, fuel cells, electrical components, etc., can solve the problems of high vanadium ion permeability, complex process and high production cost, and achieve a simple and easy preparation process. , easy environment friendly, low cost effect
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Embodiment 1
[0039] (1) Under the protection of nitrogen, after dissolving 0.02mol 4,4'-diamino-4"-hydroxytriphenylmethane in 50ml m-cresol, conduct polycondensation reaction with pyromellitic dianhydride at -10°C for 3 hours , Then add 25ml of xylene, heat up to 100°C for dehydration reaction for 3 hours to obtain compound a;
[0040] The structural formula of a is: Where R 1 for R 2 for n=50; the spectrum analysis of compound b is as follows: 1 H-NMR (DMSO-d6) "9.38 (s, OH, 1H), 8.35-6.74 (m, PhH, 14H), 5.69 (s, CH, 1H);
[0041] (2) Dissolve 0.01 mol of compound b in 20 ml of N,N-dimethylformamide, add 0.01 mol of triethylamine and 0.01 mol of 2-bromopropionyl bromide, and react at 0°C for 1 hour to obtain compound b; The structural formula of b is: Where R 1 for R 2 for n=50, R 3 for The spectrum analysis of compound b is as follows: 1 H-NMR (DMSO-d6) "8.35-6.74 (m, PhH, 14H), 5.69 (s, CH, 1H), 4.47 (s, CH, 1H), 1.90 (s, CH 3 , 3H);
[0042] (3) 0.01mol of compound b is dissolved in c...
Embodiment 2
[0052] (1) Under the protection of nitrogen, after 0.02mol 3,5-diaminophenol is dissolved in 50ml N,N-dimethylacetamide, it is mixed with 0.028mol 3,3′,4,4′-biphenyltetracarboxylic acid two The anhydride was subjected to polycondensation reaction at -5°C for 8 hours, then 25ml of xylene was added, and the temperature was raised to 120°C for dehydration reaction for 10 hours to obtain compound a; the structural formula of compound a is: Where R 1 for R 2 for n=500; the spectrum analysis of compound a is as follows: 1 H-NMR (DMSO-d6): 8.5~7.5 (m, PhH, 9H), 9.40 (s, OH, 2H);
[0053] (2) Dissolve 0.01mol of compound a in 30ml of dioxane, add 0.03mol of triethylamine and 0.03mol of 2-bromoisobutyryl bromide, react at 15°C for 3 hours to obtain compound b; the structural formula of compound b is : Where R 1 for R 2 for n=500, R 3 for The spectrum analysis of compound b is as follows: 1 H-NMR(DMSO-d6): 8.5~7.5(m, PhH, 9H), 1.98(s, CH 3 , 6H);
[0054] (3) 0.01mol of compound b is ...
Embodiment 3
[0060] (1) Under the protection of nitrogen, after 0.03mol 3,3'-diamino-4,4'-dihydroxybiphenyl is dissolved in 80ml m-cresol, and 0.045mol 3,3',4,4'-bis Phenyl ether tetracarboxylic dianhydride was subjected to polycondensation reaction at 0°C for 12 hours, then 40ml of xylene was added, and the temperature was raised to 170°C for dehydration reaction for 16 hours to obtain compound a; the structural formula of compound a is: Where R 1 for R 2 for n=3000; the spectrum analysis of compound a is as follows: 1 H-NMR (DMSO-d6) "9.35 (s, OH, 2H), 8.39-6.71 (m, PhH, 12H);
[0061] (2) Dissolve 0.02 mol of compound a in 50 ml of pyridine, add 0.1 mol of 2-bromobutyryl bromide, and react at 30°C for 7 hours to obtain compound b; the structural formula of compound b is:
[0062] Where R 1 for R 2 for n=3000, R 3 for The spectrum analysis of compound b is as follows: 1 H-NMR (DMSO-d6) "8.33-6.77 (m, PhH, 12H), 5.66 (s, CH, 1H), 4.42 (s, CH, 1H), 1.08 (s, CH 3 , 3H), 2.13 (m, CH 2 , 2H)...
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