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Production method for 2 or multi-halohydrocarbon crosslinked polybenzimidazole crosslinked membrane

A technology of polybenzimidazole and aminopolybenzimidazole, 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

AI Technical Summary

Problems solved by technology

The methods disclosed in the above patents all require high temperature (such as 300°C) cross-linking reaction. Because the cross-linking agent is easily volatile and lost at high temperature, it is difficult to accurately control the cross-linking density.

Method used

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  • Production method for 2 or multi-halohydrocarbon crosslinked polybenzimidazole crosslinked membrane
  • Production method for 2 or multi-halohydrocarbon crosslinked polybenzimidazole crosslinked membrane
  • Production method for 2 or multi-halohydrocarbon crosslinked polybenzimidazole crosslinked membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of amino-containing polybenzimidazole homopolymers from 5-aminoisophthalic acid and 3,3',4,4'-tetraaminobiphenyl:

[0035] Add 5mmol (1.071g) of 3,3',4,4'-tetraaminobiphenyl and 5mmol (0.905g) of 5-aminoisophthalic acid into 20g of polyphosphoric acid containing 70-90wt% phosphorus pentoxide , Under the condition of mechanical stirring under the protection of nitrogen, first react at 150°C for 2 hours, then react at 190°C for 20 hours, and pour into water after cooling down. First neutralize to weak acidity with sodium hydroxide, then neutralize to neutral with sodium bicarbonate, filter, put the collected polymer in ammonia water at 80°C and stir for 12 hours, filter, wash the sample to neutral, 100 °C for 24 hours in vacuum to obtain a homopolymer of amino-containing polybenzimidazole.

[0036] Its intrinsic viscosity is 0.64dL / g, Fig. 1 is its nuclear magnetic resonance spectrum, Fig. 2 is its infrared spectrum.

[0037] Preparation of 1,3-dibromopropan...

Embodiment 2

[0041] The amino-containing polybenzimidazole copolymer was prepared from 5-aminoisophthalic acid, isophthalic acid and 3,3',4,4'-tetraaminobiphenyl.

[0042]Add 6mmol (1.2856g) 3,3',4,4'-tetraaminobiphenyl, 3mmol (0.4984g) isophthalic acid and 3mmol (0.543g) 5-aminoisophthalic acid to 20g containing 70-90wt % phosphorus pentoxide polyphosphoric acid, under the condition of mechanical stirring under the protection of nitrogen, first react at 150°C for 2 hours, then react at 190°C for 20 hours, and pour it into water after cooling down to room temperature. First neutralize to weak acidity with sodium hydroxide, then neutralize to neutral with sodium bicarbonate, filter, put the collected polymer in ammonia water at 80°C and stir for 12 hours, filter, wash the sample to neutral, 100 °C for 24 hours in vacuum to obtain a copolymer containing amino polybenzimidazole. Its intrinsic viscosity is 0.36dL / g.

[0043] Preparation of polybenzimidazole cross-linked film cross-linked wit...

Embodiment 3

[0046] The amino-containing polybenzimidazole copolymer was prepared from 5-aminoisophthalic acid, isophthalic acid and 3,3',4,4'-tetraaminobiphenyl.

[0047] 6mmol (1.2856g) 3,3',4,4'-tetraaminobiphenyl, 4mmol (0.6645) isophthalic acid and 2mmol (0.362g) 5-aminoisophthalic acid were added to 20g containing 70-90wt% In the polyphosphoric acid of phosphorus pentoxide, 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 pour it into water after cooling down to room temperature. First neutralize to weak acidity with sodium hydroxide, then neutralize to neutral with sodium bicarbonate, filter, put the collected polymer in ammonia water at 80°C and stir for 12 hours, filter, wash the sample to neutral, 100 °C for 24 hours in vacuum to obtain a copolymer containing amino polybenzimidazole. Its intrinsic viscosity is 1.40dL / g.

[0048] Preparation of 1,3-dibromopropane crosslinked polybenzimidaz...

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Abstract

The invention relates to a preparation method of a polybenzimidazole crosslinking membrane that is crosslinked with bihalohydrocarbon or polyhalohydrocarbon, 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 to prepare copolymer containing 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. Both the structures of the homopolymer and the copolymer of the polybenzimidazole contain amino that can be used for crosslinking. The bihalohydrocarbon or the polyhalohydrocarbon is used as cross linking agent. The polybenzimidazole crosslinking membrane with good property can be prepared through crosslinking reaction of the amino contained in the polybenzimidazole and the bihalohydrocarbon or the polyhalohydrocarbon.

Description

technical field [0001] The invention relates to a method for preparing a polybenzimidazole cross-linked film cross-linked by two or more halogenated hydrocarbons, and prepares a high-performance halogenated hydrocarbon cross-linked film containing amino-soluble polybenzimidazole, which belongs to chemical material technology field. 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 t...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/04C08K5/02
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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