Production method for maleic anhydride modified polybenzimidazole crosslinked membrane

A technology of aminopolybenzimidazole and maleic anhydride, which is applied in the field of chemical materials, can solve the problems of easy volatilization loss of crosslinking agent and difficulty in precise control of crosslinking density, and achieve excellent mechanical properties, simple method and mild reaction conditions Effect

Inactive Publication Date: 2008-07-16
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods disclosed in the above patents all require high temperature (such as 300°C) cross-linking reaction. Because the cros

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  • Production method for maleic anhydride modified polybenzimidazole crosslinked membrane
  • Production method for maleic anhydride modified polybenzimidazole crosslinked membrane
  • Production method for maleic anhydride modified polybenzimidazole crosslinked membrane

Examples

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Example Embodiment

[0035] Example 1

[0036] Preparation of homopolymer containing amino polybenzimidazole from 5-aminoisophthalic acid and 3,3’,4,4’-tetraaminobiphenyl:

[0037] Add 5mmol (1.071g) 3,3',4,4'-tetraaminobiphenyl and 5mmol (0.905g) 5-aminoisophthalic acid to 20g polyphosphoric acid containing 70-90wt% phosphorus pentoxide , Under the condition of mechanical stirring under nitrogen protection, first react at 150°C for 2 hours, then react at 190°C for 20 hours, then pour into water after cooling. First neutralize with sodium hydroxide to weak acidity, then neutralize with sodium bicarbonate to neutrality, filter, put the collected polymer into ammonia water and stir for 12 hours at 80°C, filter, after washing the sample to neutrality, 100 Vacuum drying at °C for 24 hours to obtain an amino-containing polybenzimidazole homopolymer.

[0038] Its intrinsic viscosity is 0.64dL / g, Figure 1 is its nuclear magnetic resonance spectrum, and Figure 2 is its infrared spectrum.

[0039] Preparation ...

Example Embodiment

[0043] Example 2

[0044] From 5-aminoisophthalic acid, isophthalic acid and 3,3',4,4'-tetraaminobiphenyl to prepare copolymer containing amino polybenzimidazole:

[0045] Add 6mmol (1.2856g) 3,3',4,4'-tetraaminobiphenyl, 3mmol (0.4984) isophthalic acid and 3mmol (0.543g) 5-aminoisophthalic acid to 20g containing 70-90wt% Phosphorus pentoxide in the polyphosphoric acid, under the condition of nitrogen protection and mechanical stirring, first react at 150°C for 2 hours, then react at 190°C for 20 hours, and then pour it into water after cooling to room temperature. First neutralize with sodium hydroxide to weak acidity, then neutralize with sodium bicarbonate to neutrality, filter, put the collected polymer into ammonia water and stir for 12 hours at 80°C, filter, after washing the sample to neutrality, 100 Vacuum drying at °C for 24 hours to obtain an amino-containing polybenzimidazole copolymer. Its intrinsic viscosity is 0.36dL / g.

[0046] Preparation of maleic anhydride modifie...

Example Embodiment

[0049] Example 3

[0050] From 5-aminoisophthalic acid, isophthalic acid and 3,3',4,4'-tetraaminobiphenyl to prepare copolymer containing amino polybenzimidazole:

[0051] Add 6mmol (1.2856g) 3,3',4,4'-tetraaminobiphenyl, 4mmol (0.6645) isophthalic acid and 2mmol (0.362g) 5-aminoisophthalic acid to 20g containing 70-90wt% Phosphorus pentoxide in the polyphosphoric acid, under the condition of nitrogen protection and mechanical stirring, first react at 150°C for 2 hours, then react at 190°C for 20 hours, and then pour it into water after cooling to room temperature. First neutralize with sodium hydroxide to weak acidity, then neutralize with sodium bicarbonate to neutrality, filter, put the collected polymer into ammonia water and stir for 12 hours at 80°C, filter, after washing the sample to neutrality, 100 Vacuum drying at °C for 24 hours to obtain an amino-containing polybenzimidazole copolymer. Its intrinsic viscosity is 1.40dL / g.

[0052] Preparation of maleic anhydride modifi...

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Abstract

The invention relates to a preparation method of a maleic anhydride modified polybenzimidazole crosslinking membrane, which takes amino dibasic acid and aromatic tetraamine as monomer raw material and polyphosphoric acid as reaction medium and reaction is carried out for 5-30 hours at 150-220 DEG C under the nitrogen protection condition so as to obtain homopolymer containing amino polybenzimidazole, and takes the amino dibasic acid, nonaminonic dibasic acid and the aromatic tetraamine as the monomer raw materials so as to prepare copolymer of amino polyphosphoric under the same conditions. The prepared homopolymer and the copolymer of the polybenzimidazole have good dissolvability in solvents of dimethyl sulphoxide, N, N- dimethylacetamide, phosphate, vitriol and methane-sulforic acid, etc. and after the prepared homopolymer and the copolymer of the polybenzimidazole are dissolved in an organic solvent, reaction is carried out with the maleic anhydride to obtain maleic anhydride modified polybenzimidazole which goes through thermal crosslinking when casting into membrane, thereby obtaining the polybenzimidazole crosslinking membrane that has good mechanical property.

Description

technical field [0001] The invention relates to a method for preparing a maleic anhydride-modified polybenzimidazole cross-linked film, and prepares a high-performance maleic anhydride cross-linked film containing amino-soluble polybenzimidazole, which belongs to the technical field of chemical materials. Background technique [0002] The polybenzimidazole with full aromatic structure is a kind of high-performance material, which has extremely high heat resistance, excellent 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 prospects in the field of high-temperature proton exchange membrane fuel cells. Therefore, this type of material has received great attention in recent years. However, due to the high rigidity of polyb...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L51/08
Inventor 房建华徐楠张桂梅郭晓霞徐宏杰印杰
Owner SHANGHAI JIAO TONG UNIV
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