Method for preparing polybenzimidazole cross-link membranes from functionalized graphene oxide
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A polybenzimidazole, functionalized technology, used in electrochemical generators, fuel cells, electrical components, etc., can solve the problems of low membrane mechanical strength, phosphoric acid leakage, etc., and achieve uniform size, mild reaction, and high yield. Effect
Inactive Publication Date: 2018-01-23
JIANGNAN GRAPHENE RES INST
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[0004] The technical problem mainly solved by the present invention is the low mechanical strength of the
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Embodiment 1
[0024] Embodiment 1: Preparation of the homopolymer (PBI) of polybenzimidazole:
[0025] Preparation of homopolymer of polybenzimidazole with isophthalic acid and 3,3',4,4'-tetraaminobiphenyl: 12.460g (75 mmol) of isophthalic acid, 3,3',4,4' - Add 16.074 g (75 mmol) of tetraaminobiphenyl to 300 g polyphosphoric acid containing 70-90wt% phosphorus pentoxide, stir mechanically under nitrogen protection, heat the mixture at 190°C for 5 hours with a temperature-controlled heating device, and cool down Then pour into the water. First use sodium hydroxide to neutralize to weak acidity, then use sodium bicarbonate to neutralize to neutral, filter, put the collected polymer in ammonia water at 80°C and stir for 12 hours, filter, wash the sample to neutral, 110 °C for 24 hours in vacuum to obtain a homopolymer of polybenzimidazole.
Embodiment 2
[0026] Embodiment 2: the preparation of graphene oxide (GO):
[0027] Take 10 g (325 mesh) flake graphite and 250 mL of 98% concentrated sulfuric acid and mix evenly, then add 10.0 g of potassium nitrate, quickly add 60 g of potassium permanganate in a water bath at 15 °C, and mix evenly. Then raise the temperature of the system to 40 °C, add 300 mL of water after 3 h of reaction, and at the same time raise the temperature of the system to 80 °C for 30 min, then reduce the excess potassium permanganate with 250 mL of distilled water and 100 mL of hydrogen peroxide (30wt%) , centrifuged and washed to pH 5, diluted to 0.1 g / L with deionized water, and the suspension was sonicated at a frequency of 10 kHz for 1 h to achieve monolayer exfoliation and obtain a uniform and stable graphene oxide dispersion. Graphene oxide powder was obtained after freeze-drying for 6 h.
[0029] Prepare the hydrolyzate of silane coupling agent KH560 with silane coupling agent KH560, methanol, glycerol and water at a mass ratio of 10:10:1:79, adjust the pH to 1 with diluted nitric acid solution, and hydrolyze at 20°C for 1 h , add graphene oxide (GO) powder, the mass ratio of silane to graphene oxide powder is 0.1:1, after ultrasonic dispersion for 1 h, react at 40°C for 6 h, wash with methanol and water, and freeze-dry for 72 h to obtain KH560 -GO;
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Abstract
The invention relates to a method for preparing polybenzimidazole cross-link membranes from functionalized graphene oxide. The polybenzimidazole cross-link membranes comprise polybenzimidazole homopolymers, modified graphene oxide and phosphoric acid. The method has the advantages that binary acid and aromatic quaternary amine are used as monomer raw materials, polyphosphoric acid is used as a reaction medium, reaction is carried out at the temperature of 150-220 DEG C under the condition of nitrogen protection for 5-30 h to obtain the polybenzimidazole homopolymers, and the prepared polybenzimidazole homopolymers in solvents such as dimethyl sulfoxide, N, N-dimethylacetamide, phosphoric acid, sulfuric acid and methylsulfonic acid are excellent in dissolubility; graphene oxide (GO) powderis prepared by the aid of improved Hummers processes, and graphene oxide is modified by the aid of silane coupling agents (KH560) to obtain the functionalized graphene oxide (KH560-GO); the prepared functionalized graphene oxide (KH560-GO) is used as a cross-linking agent, and the polybenzimidazole cross-link membranes with excellent mechanical performance and methanol diffusion resistance can beprepared by the aid of cross-linking reaction between imidazole rings in the prepared polybenzimidazole homopolymers and epoxy functional groups in the functionalized graphene oxide (KH560-GO); cross-link membranes can be ultimately soaked in phosphoric acid solution (with the concentration of 50-85%) for 6-24 h to obtain the polybenzimidazole cross-link membranes with low phosphoric acid doping,and service requirements in the field of high-temperature fuel cells, sensors and the like can be met.
Description
technical field [0001] The invention relates to a method for preparing a polybenzimidazole cross-linked film from functionalized graphene oxide, and prepares a high-performance polybenzimidazole cross-linked film by using graphene oxide functionalized with a silane coupling agent as a cross-linking agent , can be used in polymer membrane fuel cells (including PEMFC, DMFC), can also be used in high-temperature electrolysis, sensors and other fields, can also be used in the field of solid acid catalysts, and belongs to the technical field of chemical materials. Background technique [0002] Polybenzimidazole has extremely high heat resistance, excellent high-temperature mechanical properties, excellent chemical stability, good dielectric properties and spinning and film-forming properties. It has been widely used in aerospace, microelectronics and other fields. In the mid-1990s, it was discovered that polybenzimidazole doped with phosphoric acid has potential application pros...
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