Crosslinked polybenzimidazoles thin film containing sulfonic group and preparation thereof

A polybenzimidazole and sulfonic acid group-containing technology, applied in the field of polybenzimidazole films and their preparation, can solve the problems of difficult processing, difficult monomer synthesis, poor film-forming properties and mechanical properties, etc., and achieve good transparency , the effect of excellent solubility, high thermal stability

Inactive Publication Date: 2009-07-15
BEIJING INSTITUTE OF GRAPHIC COMMUNICATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with linear polymers, although hyperbranched polymers have the advantages of good solubility and easy processing, their film-forming properties and mechanical properties are poor, so they are often processed by cross-linking, blending or tooling. Improve the properties of materials
At present, there are few literature reports on the synthesis and application of hyperbranched fully aromatic polybenzimidazoles. The main reason is that the monomers are difficult to synthesize and difficult to process [ZX Li, JH Liu, SY Yang, et.al.Synthesis and characterization of novel hyperbranched polybenzimidazoles based on an AB 2 monomer containing four amino groups and one carboxylic group, J Polym SciPart A: Polym Chem 2006, 44, 5729-5739.]

Method used

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  • Crosslinked polybenzimidazoles thin film containing sulfonic group and preparation thereof
  • Crosslinked polybenzimidazoles thin film containing sulfonic group and preparation thereof
  • Crosslinked polybenzimidazoles thin film containing sulfonic group and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Dissolve 4.60g of 3,3',4,4'-tetraaminodiphenyl ether and 4.60g of aromatic triacid A1 (see page 4 for the structure) in 138g of polyphosphoric acid (content: 83%) , a transparent homogeneous solution was obtained. Under nitrogen protection, the above solution was heated at 160° C. for 5 h, and then heated to 180° C. for 3 h to obtain a viscous solution. Cool to room temperature and pour into 500ml of water. The precipitate was collected and washed with 5% by weight NaOH aqueous solution, then hot distilled water until neutral to obtain a beige solid. The light brown solid was dried under vacuum at 60° C. for 10 hours to obtain 7.60 g of branched polybenzimidazole (HPBI-1) with a yield of 94%. Intrinsic viscosity 0.46dL / g (0.5g / dL NMP solution, 25°C).

[0045] 7.60 g of HPBI-1, 0.92 g of 1,2-naphthoquinone-4-ammonium sulfonate and 0.92 g of polyether benzil PEB-1 (see page 5 for the structure; number average molecular weight 11,723; repeating unit The molecular weigh...

Embodiment 2

[0047] Dissolve 4.60g of 3,3',4,4'-tetraaminodiphenyl ether and 2.3g of aromatic triacid A2 (see page 4 for the structure) in 92g of polyphosphoric acid (content: 83%) , a transparent homogeneous solution was obtained. Under nitrogen protection, the above solution was heated at 160° C. for 5 h, and then heated to 180° C. for 11 h to obtain a viscous solution. Cool to room temperature and pour into 500ml of water. The precipitate was collected and washed with 5% by weight NaOH aqueous solution, then hot distilled water until neutral to obtain a beige solid. The light brown solid was dried under vacuum at 60° C. for 10 hours to obtain 6.32 g of branched polybenzimidazole (HPBI-2) with a yield of 95%. Intrinsic viscosity 0.40dL / g (0.5g / dL NMP solution, 25°C).

[0048] 6.32 g of HPBI-2, 1.38 g of 1,2-naphthoquinone-4-ammonium sulfonate and 0.23 g of polyether benzil PEB-1 (number average molecular weight 11,723; repeating unit molecular weight is 434.5) were dissolved in 46 g ...

Embodiment 3

[0050] 4.60g of 3,3',4,4'-tetraaminodiphenyl ether and 2.12g of aromatic triacid A1 and 2.13g of aromatic triacid A2 are dissolved in 120g of polyphosphoric acid (content is 83%) to obtain Transparent homogeneous solution. Under nitrogen protection, the above solution was heated at 160° C. for 3 h, and then heated to 180° C. for 3 h to obtain a viscous solution. Cool to room temperature and pour into 500ml of water. The precipitate was collected and washed with 5% by weight NaOH aqueous solution, then hot distilled water until neutral to obtain a beige solid. The light brown solid was dried under vacuum at 60° C. for 10 hours to obtain 7.28 g of branched polybenzimidazole (HPBI-3) with a yield of 94%. Intrinsic viscosity 0.44dL / g (0.5g / dL NMP solution, 25°C).

[0051]7.28 g of HPBI-3, 1.25 g of 1,2-naphthoquinone-4-ammonium sulfonate and 0.55 g of polyether benzil PEB-2 (see page 5 for the structure; number average molecular weight 11,516; repeating unit The molecular weig...

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Abstract

The invention relates to a crosslinked polybenzimidazole film containing sulfo group and a method for preparing the same. The invention is characterized in that the raw material proportions of the crosslinked polybenzimidazole film are as follows: (1) 10 proportions of 3,3',4,4'-tetraamino diphenyl ether by weight; (2) 5-10 proportions of aromatic triacid by weight; (3) 2-3 proportions of 1,2-naphthoquinone-4-ammonium sulphonate by weight; (4) 0.5-2 proportions of PEB by weight; (5) 100-200 proportions of organic solvent by weight; and (6) 200-300 proportions of polyphosphoric acid by weight. The film can effectively regulate the molecular weight of the branched polybenzimidazole and the structure of the crosslinked film by controlling the raw material proportions. The obtained polybenzimidazole has excellent solubility as well as higher thermal stability, better transparence, excellent corrosion resistance and high proton conduction rate, and the like.

Description

technical field [0001] The invention relates to a polybenzimidazole film and a preparation method thereof, in particular to a cross-linked polybenzimidazole film containing sulfonic acid groups and a preparation method thereof. Background technique [0002] As a kind of aromatic heterocyclic polymer, polybenzimidazole has excellent heat resistance, low temperature resistance, self-lubricating property, radiation resistance, hydrolysis resistance, flame retardant and ablation resistance, etc. Excellent mechanical properties and dielectric properties, etc., especially suitable as high-temperature resistant fibers, adhesives, structural materials and functional materials, have been successfully used in radome, fairing and empennage of medium and hypersonic aircraft, ablation resistance Coatings, printed circuit boards, spacecraft radiation-resistant materials, C-class electrical insulation materials, and FPC substrates in the field of electronics and microelectronics, etc. [(a)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/18C08J3/24C08J5/18C08J5/22
Inventor 李仲晓蒲嘉陵韦韦
Owner BEIJING INSTITUTE OF GRAPHIC COMMUNICATION
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