Polybenzimidazole film with nanometer porous structure and preparation method thereof

A polybenzimidazole membrane and polybenzimidazole technology are applied in the field of polybenzimidazole membrane and its preparation, which can solve the problems of inability to accurately control the size and distribution of pores, decrease in proton conductivity, loss of phosphoric acid, etc., and achieve ultra-fast Phosphoric acid adsorption rate, excellent stability, effect of large internal space

Active Publication Date: 2019-01-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And commonly used organic small molecule porogens such as dimethyl phthalate, diethyl phthalate, dibutyl phthalate, diphenyl phthalate, triphenyl phosphate often get When the polybenzimidazole membrane has a high porosity, the pore size is on the order of

Method used

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  • Polybenzimidazole film with nanometer porous structure and preparation method thereof
  • Polybenzimidazole film with nanometer porous structure and preparation method thereof
  • Polybenzimidazole film with nanometer porous structure and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1) Ultrasonically disperse ZIF-8 nanoparticles with a size of about 100nm in DMAc, and add them to the DMAc solution of OPBI. The mass ratio of ZIF-8 and OPBI is 2:8, ultrasonically disperse and stir vigorously to make the two evenly mixed, Use a 400-mesh filter cloth to filter out impurities, cast it on a clean glass plate, dry it in a vacuum oven at 80°C for 12 hours, at 100°C for 12 hours, at 120°C for 12 hours, and finally vacuumize and keep it at 120°C for 12 hours to obtain polybenzone imidazole film.

[0030] 2) Soak the obtained polybenzimidazole film in 85% (wt) phosphoric acid at 120°C for 24h, then wash with boiling water for 5h to remove residual etchant, and dry at 120°C for 12h; repeat the above washing and drying process twice, A polybenzimidazole membrane with a nanoporous structure is obtained.

[0031] The polybenzimidazole film of the nanoporous structure obtained in the present embodiment has been carried out scanning electron microscope characteriz...

Embodiment 2

[0034] 1) Ultrasonically disperse ZIF-8 nanoparticles with a size of about 150nm in DMAc, and add them to the DMAc solution of OPBI. The mass ratio of ZIF-8 and OPBI is 2:8, ultrasonically disperse and stir vigorously to make the two evenly mixed, Use a 400-mesh filter cloth to filter out impurities, cast it on a clean glass plate, dry it in a vacuum oven at 80°C for 12 hours, at 100°C for 12 hours, at 120°C for 12 hours, and finally vacuumize and keep it at 120°C for 12 hours to obtain polybenzone imidazole film.

[0035] 2) Soak the obtained polybenzimidazole membrane in 85% (wt) phosphoric acid at 120°C for 12h, then wash with boiling water for 5h to remove residual etchant, and dry at 120°C for 12h to obtain polybenzoimidazole with nanoporous structure. The imidazole membrane has a pore size of about 850nm. The phosphoric acid doping level at 120°C for 24 hours can reach 25, and the proton conductivity of the doped phosphoric acid film at 200°C for 24 hours is 115mS / cm. ...

Embodiment 3

[0037] 1) Ultrasonically disperse ZIF-8 nanoparticles with a size of about 200nm in DMAc, and add them to the DMAc solution of OPBI. The mass ratio of ZIF-8 and OPBI is 1:9, ultrasonically disperse and stir vigorously to make the two evenly mixed. Use a filter cloth to filter out impurities, cast on a clean glass plate, dry in a vacuum oven at 80°C for 12h, at 100°C for 12h, at 120°C for 12h, and finally vacuumize and keep at 120°C for 12h to obtain a polybenzimidazole film .

[0038] 2) Soak the obtained polybenzimidazole membrane in 85% (wt) phosphoric acid at 120°C for 24h, then wash with boiling water for 5h to remove residual etchant, and dry at 120°C for 12h to obtain polybenzoimidazole with nanoporous structure. The imidazole membrane has a pore size of about 750nm. The phosphoric acid doping level at 120°C for 24 hours can reach 23, and the proton conductivity of the doped phosphoric acid film at 200°C for 24 hours is 100mS / cm.

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Abstract

The invention relates to a polybenzimidazole film with a nanometer porous structure and a preparation method thereof and belongs to the technical field of special macromolecular functional films. Thepreparation method comprises the following steps: adding filler dispersion liquid into a polybenzimidazole solution, fully mixing and filtering, and then pouring onto a clean glass plate; heating andremoving solvent, thereby acquiring a polybenzimidazole film on the glass plate; soaking for a period of time in an etching agent; washing with boiled water and removing residual etching agent; drying, thereby acquiring the polybenzimidazole film with the nanometer porous structure. The polybenzimidazole film has high phosphoric acid doped level and high proton conductivity and can be applied to high-temperature fuel cells. According to the invention, a zeolite imidazate framework ZIFs series of materials are taken as pore-foaming agents and phosphoric acid is taken as the etching agent so asto in situ form the nanometer porous structure in the polybenzimidazole film. ZIFs materials can acquire different crystal sizes and morphologies by adjusting the molecular structure of imidazole ligand and the type of metal ions, so that the pore size, pore morphology, pore size distribution and pore connectivity of the prepared porous film all can be regulated.

Description

technical field [0001] The invention belongs to the technical field of special polymer functional membranes, and specifically relates to a polybenzimidazole membrane with a nanoporous structure and a preparation method thereof. Background technique [0002] Nanoporous polymer membranes have the characteristics of large specific surface area, low density, high stability and good processability, and have the dual advantages of porous membranes and polymer materials. The field of battery proton exchange membrane has a wide range of applications. However, the porous polymer membrane prepared by the current method has the problems of wide pore size distribution, uncontrollable pore size, cumbersome preparation process and environmental pollution caused by waste discharge. [0003] Polybenzimidazole is a class of heterocyclic ladder polymers containing imidazole groups in the main chain repeating unit, which has excellent stability, mechanical strength, and chemical corrosion res...

Claims

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Application Information

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IPC IPC(8): C08L79/04C08L87/00C08J5/22
CPCC08J5/2256C08J2379/04C08J2487/00
Inventor 刘佰军张留夫王鹏李天洋
Owner JILIN UNIV
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