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Preparation method of branched-cross-linked sulfonated polyimide membrane

A technology of sulfonated polyimide membrane and benzidine bissulfonate, applied in the field of battery separator, can solve the problems of insufficient chemical stability of SPI membrane materials, improve interaction and space free volume, and solve the problem of proton conductivity. Lower, enhance the effect of vanadium resistance

Active Publication Date: 2021-10-29
SOUTHWEAT UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, when the branched structure is introduced into SPI, it can also greatly improve the performance of VRFB, but the chemical stability of the SPI membrane material prepared by the prior art is not good enough.

Method used

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  • Preparation method of branched-cross-linked sulfonated polyimide membrane
  • Preparation method of branched-cross-linked sulfonated polyimide membrane
  • Preparation method of branched-cross-linked sulfonated polyimide membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of branched-crosslinked sulfonated polyimide membrane, comprising the following steps:

[0037] Step 1. Under nitrogen protection, add 8.0mmol benzoic acid, 20mL m-cresol Ⅰ, and 4.0mmol NTDA into a 250mL three-necked flask, and stir at 60°C until the solid is completely dissolved; then, add 2.0mmol BDSA, 20mL m-cresol Put cresol Ⅱ and 2.6mL triethylamine in a beaker, stir at 60°C until the solid is completely dissolved, then add 0.4mmol TFAPOB, 0.92mmol ODA and 0.24mmol BTA, and slowly dissolve the solution with a constant pressure funnel after the solid is completely dissolved. Add it dropwise into the above-mentioned three-necked flask, and stir and react at 60°C for 15 hours to obtain a branched-crosslinked sulfonated polyimide casting solution; pour the casting solution onto a dry and clean glass plate to form a film, Dry at 60°C for 15 hours; dry at 80°C, 100°C, 120°C, and 150°C for 1 hour each to obtain a triethylamine salt-type branched-cross...

Embodiment 2

[0041] A preparation method of branched-crosslinked sulfonated polyimide membrane, comprising the following steps:

[0042] Step 1. Under nitrogen protection, add 8.0mmol benzoic acid, 20mL m-cresol Ⅰ, and 4.0mmol NTDA into a 250mL three-necked flask, and stir at 60°C until the solid is completely dissolved; then, add 2.0mmol BDSA, 20mL m-cresol Put cresol Ⅱ and 2.6mL triethylamine in a beaker, stir at 60°C until the solids are completely dissolved, then add 0.4mmol TFAPOB, 0.76mmol ODA and 0.32mmol BTA, and slowly dissolve the solution with a constant pressure funnel after the solids are completely dissolved. Add it dropwise into the above-mentioned three-necked flask, and stir and react at 60°C for 12 hours to obtain a branched-crosslinked sulfonated polyimide casting solution; pour the casting solution onto a dry and clean glass plate to form a film, Dry at 60°C for 15 hours; dry at 80°C, 100°C, 120°C, and 150°C for 1 hour each to obtain a triethylamine salt-type branched-c...

Embodiment 3

[0046] A preparation method of branched-crosslinked sulfonated polyimide membrane, comprising the following steps:

[0047] Step 1. Under nitrogen protection, add 8.0mmol benzoic acid, 20mL m-cresol Ⅰ, and 4.0mmol NTDA into a 250mL three-necked flask, and stir at 60°C until the solid is completely dissolved; then, add 2.0mmol BDSA, 20mL m-cresol Put cresol Ⅱ and 2.6mL triethylamine in a beaker, stir at 60°C until the solid is completely dissolved, then add 0.4mmol TFAPOB, 0.6mmol ODA and 0.4mmol BTA, and slowly drop the solution using a constant pressure funnel after the solid is completely dissolved Add it into the above-mentioned three-necked flask, and stir and react at 60°C for 10 hours to obtain a branched-crosslinked sulfonated polyimide casting solution; pour the casting solution on a dry and clean glass plate to form a film, and Dry at 60°C for 15 hours; dry at 80°C, 100°C, 120°C, and 150°C for 1 hour each to obtain a triethylamine salt-type branched-crosslinked sulfon...

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Abstract

The invention discloses a preparation method of a branched-crosslinked sulfonated polyimide membrane. A novel branched-crosslinked polyimide membrane material is prepared from a Y-type branched triamine monomer, an X-type crosslinked tetramine monomer, a sulfonated diamine monomer, a non-sulfonated diamine monomer and an anhydride monomer through film casting and high-temperature polymerization methods. The Y-type branched monomer and the X-type cross-linked tetramine monomer are both self-synthesized. The molar ratio of the cross-linked tetramine to the non-sulfonated diamine to the anhydride to the branched triamine to the sulfonated diamine to benzoic acid is (0.06-0.14): (0.07-0.23): 1: 0.1: 0.5: 2. The cross-linking degree of the separator membrane can be controlled by regulating and controlling the proportion of the dosage of the cross-linking monomers. By introducing the branched cross-linked structure, the stability and vanadium resistance of the membrane can be effectively improved, and the efficiency and the service lifetime of the all-vanadium redox flow battery can be effectively improved. In conclusion, the branched-cross-linked sulfonated polyimide membrane prepared by the method has a good application prospect in the field of all-vanadium redox flow batteries.

Description

technical field [0001] The invention belongs to the field of battery separators, and relates to a preparation method of a branched-crosslinked sulfonated polyimide membrane. Background technique [0002] With the continuous development of the economy, more and more attention has been paid to the utilization of renewable energy, so energy storage and conversion systems need to play a vital role in energy applications. All-vanadium redox flow battery (VRFB) is an excellent energy storage system, which has many advantages such as fast response, long life, good reliability, and strong deep discharge capability. As one of the important component materials of VRFB, proton exchange membrane (PEM) can separate positive and negative electrolytes to avoid cross-contamination of vanadium ions and conduct protons to make the battery form a loop. Therefore, PEM should have high proton conductivity, excellent vanadium resistance and outstanding chemical stability. So far, the Nafion mem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J7/12C08J7/14C08G73/10C08L79/08
CPCC08J5/18C08J7/12C08J7/14C08G73/1071C08G73/1085C08J2379/08Y02E60/50
Inventor 李劲超张亚萍刘军胥文杰罗钢黄文恒龙俊罗欢
Owner SOUTHWEAT UNIV OF SCI & TECH
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