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Preparation of side-chained sulfonated polyimide of which main chain contains quinoxaline perssad and application of side-chained sulfonated polyimide

A technology of sulfonated polyimide and sulfonated polyimide copolymer, which is applied in the preparation of proton exchange membranes and the preparation of side chain type sulfonated polyimides, can solve the problem that is not conducive to enhancing the flexibility of polymer chains and other problems, to achieve good hydrolytic stability, high proton conductivity, high molecular weight effect

Inactive Publication Date: 2018-02-23
南京黑泰催化剂有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature (Journal of Power Sources 2011, 196, 1694) reported a preparation method of a proton exchange membrane using quinoxaline as a crosslinking group, wherein the quinoxaline structure was introduced into the side chain of the polymer, resulting in the side chain The chain structure is not conducive to enhancing the flexibility of the polymer chain

Method used

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  • Preparation of side-chained sulfonated polyimide of which main chain contains quinoxaline perssad and application of side-chained sulfonated polyimide
  • Preparation of side-chained sulfonated polyimide of which main chain contains quinoxaline perssad and application of side-chained sulfonated polyimide
  • Preparation of side-chained sulfonated polyimide of which main chain contains quinoxaline perssad and application of side-chained sulfonated polyimide

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preparation example Construction

[0044] The present invention also proposes a preparation method of a side chain type sulfonated polyimide whose main chain contains a quinoxaline group, including a preparation method of a sulfonated polyimide homopolymer (y=1) and a sulfonated polyimide The preparation method of imide copolymer (0figure 1 Shown, wherein, the preparation method of described sulfonated polyimide homopolymer (y=1) comprises the following steps:

[0045] Under the protection of nitrogen, dissolve sulfonated diamine and a certain amount of organic weak base in an organic solvent, then add dianhydride monomer and a certain amount of organic weak acid in equimolar amounts to the sulfonated diamine, and heat the reaction system at 80-140°C React for 1-8h, then react at 160-220°C for 8-24h, after the reaction, lower the temperature of the system to 70-120°C, and then pour it into methanol to obtain a filamentous product, which is dried in a vacuum oven after repeated washing Dry, obtain described sulf...

Embodiment 1

[0051] Example 1: Synthesis of a side chain type sulfonated polyimide homopolymer containing a quinoxaline group in the main chain and preparation of a proton exchange membrane:

[0052] Under the protection of nitrogen and mechanical stirring, add 4-[2,3-bis(4-aminophenyl)-quinoxaline-6-oxyl]-3,4'- Disulfonate biphenyl 6.401g (10mmol), triethylamine 2.024-4.048g (20-40mmol) and m-cresol 45-115mL, preferably, the optimal addition amount in the present embodiment is respectively 3.036g (30mmol ) and 75mL. After completely dissolving, add 1,4,5,8-naphthalene tetracarboxylic dianhydride (10mmol) 2.682g and benzoic acid 1.221-3.664g (10-30mmol), preferably, the optimal addition amount in this embodiment is 2.907 g (23.8 mmol). Under the protection of nitrogen, first raise the temperature of the reaction system to 80-140°C for 1-8h, and then continue to heat up to 160-220°C for 8-24h. Preferably, the two temperatures in this example are 100°C and 180°C respectively. ℃, the two t...

Embodiment 2

[0054] Embodiment 2: the preparation of a kind of main chain type sulfonated polyimide copolymer of side chain type sulfonated polyimide containing quinoxaline group and the preparation of proton exchange membrane:

[0055] Under the protection of nitrogen and mechanical stirring, add 4-[2,3-bis(4-aminophenyl)-quinoxaline-6-oxyl]-3,4'- Disulfonic acid biphenyl 3.201g (5mmol), the optimal addition amount of triethylamine in the present embodiment is respectively 1.619g (16mmol), m-cresol is 60mL. After dissolving completely, add 4,4'-diaminodiphenyl ether 1.001g (5mmol), 1,4,5,8-naphthalene tetracarboxylic dianhydride 2.682g (10 mmol), the maximum amount of benzoic acid in the present embodiment The optimum dosage is 2.198g (18mmol).

[0056] All the other experimental procedures were the same as in Example 1.

[0057] The preparation method of the proton exchange membrane is the same as in Example 1.

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Abstract

The invention discloses side-chained sulfonated polyimide of which a main chain contains quinoxaline perssad, a preparing method of side-chained sulfonated polyimide, and a method for applying side-chained sulfonated polyimide to prepare a protocol exchange membrane. Side-chained sulfonated polyimide is structurally characterized in that the main chain contains the quinoxaline perssad, and ether bonds or thioether bonds on side-chained sulfonated polyimide serve as connection perssad of a side chain, the flexibility of the side chain and the hydrophobicity of the main chain are guaranteed, andmeanwhile, side-chained sulfonated polyimide has high molecular weight, excellent heat stability and high hydrolytic stability. The preparing technology is simple, the reaction condition is easy to operate and control, and side-chained sulfonated polyimide is applicable to industrialized production. The protocol exchange membrane which is prepared through side-chained sulfonated polyimide of which the main chain contains the quinoxaline perssad has high protonic electric conductivity and excellent mechanical performance, and has a good application prospect.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for preparing a side chain type sulfonated polyimide whose main chain contains quinoxaline groups and a method for preparing a proton exchange membrane. Background technique [0002] Sulfonated polyimide is considered to be a promising material for proton exchange membrane fuel cells because of its good physical and chemical stability, heat resistance, high proton conductivity, easy preparation and low price. However, the imide rings of such polymers are vulnerable to nucleophilic attack, resulting in poor hydrolytic stability. Generally, the water resistance can be improved by changing the monomer structure, among which the introduction of side chain type sulfonated diamine monomer is a very effective method. Literature (ECSTransactions 2008, 12, 5) reported a side-chain sulfonated polyimide linked by ether linkages. This polymer has excellent hydrolytic stability (mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/22C08L79/08
CPCC08G73/1067C08J5/2256C08J2379/08
Inventor 王卫霞陈康成翟凤霞房建华
Owner 南京黑泰催化剂有限公司
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