Long-lateral-chain quaternarized polybenzimidazole cross-linked membrane and preparation method therefor
A polybenzimidazole and quaternization technology, applied in the chemical field, can solve problems such as reducing proton conductivity, and achieve the effects of excellent charge-discharge performance, good cycle stability and low self-discharge rate.
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Embodiment 1
[0039] Step 1) Synthesis of Monoquaternary Ammonium Salt Intermediate B:
[0040]In a 100 mL dry and clean three-necked flask, add 75 mL of toluene and 75 mL of acetonitrile in sequence, stir magnetically under nitrogen protection until completely mixed, then add 25.8 g of N,N,N',N'-tetramethyl -1,6-Hexanediamine and 2.475 g of 1-bromo-n-hexane, stirred at room temperature for 30 min, then heated to 70 °C for reaction, after 12 h, the reaction was completed, and cooled to room temperature. The mixed solvent of toluene and acetonitrile was removed by vacuum distillation, and the product was repeatedly washed with petroleum ether 3 times, and the upper liquid was separated each time, and the unreacted N,N,N',N'-tetrafluoroethylene was recovered by vacuum distillation again. Methyl-1,6-hexanediamine. The light yellow liquid in the lower layer is the reaction product B, and the yield is 91%. The proton NMR spectrum of the product (solvent: DMSO-d6) is as figure 1 As shown, the ...
Embodiment 2
[0050] Step 1) ~ step 2) are the same as in Example 1;
[0051] Step 3) Synthesis of a long side chain quaternized polybenzimidazole NH2PBI-D (1:0.6):
[0052] Under the protection of nitrogen, 0.2 g polybenzimidazole containing side amino groups (H2N-PBI) and 5 mL dimethyl sulfoxide (DMSO) solvent were successively added to a 100 mL dry and clean three-necked flask, and after magnetic stirring for 30 min, the temperature was raised to About 80 ° C, after the polymer is completely dissolved, cool to room temperature, add 0.1917 g of quaternary ammonium salt D prepared in step 2 of Example 1, continue stirring for 30 min under nitrogen protection, then heat up to 80 ° C, and at this temperature Under reaction for 10 h. After cooling to room temperature, pour the highly viscous solution in the reaction bottle into 50 mL of acetone, wash the precipitated polymer three times with acetone, and dry it under vacuum at 50°C for 10 h to prepare a long side chain quaternary ammonium P...
Embodiment 3
[0056] Step 1) ~ step 2) are the same as in Example 1;
[0057] Step 3) Synthesis of a long side chain quaternized polybenzimidazole NH2PBI-D (1:1):
[0058] Under the protection of nitrogen, 0.2 g polybenzimidazole containing side amino groups (H2N-PBI) and 5 mL dimethyl sulfoxide (DMSO) solvent were successively added to a 100 mL dry and clean three-necked flask, and after magnetic stirring for 30 min, the temperature was raised to About 80 ° C, after the polymer is completely dissolved, cool to room temperature, add 0.3195 g of quaternary ammonium salt D prepared in step 2 of Example 1, continue stirring for 30 min under nitrogen protection, then heat up to 80 ° C, and at this temperature Under reaction for 10 h. After cooling to room temperature, pour the highly viscous solution in the reaction bottle into 50 mL of acetone, wash the precipitated polymer three times with acetone, and dry it under vacuum at 60°C for 12 h to prepare a long side chain quaternary ammonium Pol...
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