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Preparation method of sulfonated polyimide/titanium dioxide composite proton conductive membrane

A technology of sulfonated polyimide and proton conductive membrane is applied in the field of preparation of battery separator, which can solve the problems of affecting the long-term service life of the battery, poor anti-oxidation ability of the separator, and decreased battery capacity, etc., and achieves good application prospects and superior chemical properties. , Excellent effect of open circuit voltage

Active Publication Date: 2013-09-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, similar to most single non-fluorine polymer proton-conducting membranes, the separator has poor oxidation resistance and is easily oxidized by the V5+ solution in the battery, resulting in microscopic defects in the membrane, causing the battery capacity to decrease due to the mixture of positive and negative electrolytes, and greatly Affects long-term battery life

Method used

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  • Preparation method of sulfonated polyimide/titanium dioxide composite proton conductive membrane
  • Preparation method of sulfonated polyimide/titanium dioxide composite proton conductive membrane

Examples

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Embodiment 1

[0026] A preparation method of sulfonated polyimide / titanium dioxide composite proton conductive membrane:

[0027] Under N2 protection, 1.0 mmol BDSA, 10 mL m-cresol, 2.0 mmol triethylamine were added to a 100 mL three-necked flask, and stirred continuously at room temperature until BDSA was completely dissolved, then 2.0 mmol NTDA, 0.49 g benzoic acid and 1.0 mmol ODA were added, After continuing to stir for a few minutes, the temperature of the system was raised to 80 °C for 4 hours, and then to 180 °C for 20 hours, and the heating was stopped to obtain a viscous polymer solution. When the temperature drops below 80 °C, add 5 mL of m-cresol to dilute the reaction solution, continue to stir for a few minutes, then pour acetone into it to obtain a flocculent polymer precipitate, filter it, and wash the precipitate repeatedly with acetone several times to remove the residual solvent and unreacted substances, and then dried at 80°C for 20 hours;

[0028]Dissolve the obtained t...

Embodiment 2

[0032] A preparation method of sulfonated polyimide / titanium dioxide composite proton conductive membrane:

[0033] Under the protection of N2, add 1.2 mmol BDSA, 10 mL m-cresol, 2.4 mmol triethylamine to a 100 mL three-necked flask, stir continuously at room temperature until BDSA is completely dissolved, add 2.0 mmol NTDA, 0.49 g benzoic acid and 0.8 mmol ODA, After continuing to stir for a few minutes, the temperature of the system was raised to 80 °C for 4 hours, and then to 180 °C for 20 hours, and the heating was stopped to obtain a viscous polymer solution. When the temperature drops below 80 °C, add 5 mL of m-cresol to dilute the reaction solution, continue to stir for a few minutes, then pour acetone into it to obtain a flocculent polymer precipitate, filter it, and wash the precipitate repeatedly with acetone several times to remove the residual solvent and unreacted substances, and then dried at 80°C for 20 hours;

[0034] Dissolve the obtained triethylamine salt-t...

Embodiment 3

[0038] A preparation method of sulfonated polyimide / titanium dioxide composite proton conductive membrane:

[0039] Under N2 protection, add 1.0 mmol BDSA, 10 mL m-cresol, 2.0 mmol triethylamine to a 100 mL three-necked flask, stir continuously at room temperature until BDSA is completely dissolved, add 2.0 mmol NTDA, 0.49 g benzoic acid and 1.0 mmol ODA, continue After stirring for a few minutes, the temperature of the system was raised to 80 °C for 4 hours, and then to 180 °C for 20 hours, and the heating was stopped to obtain a viscous polymer solution. When the temperature drops below 80 °C, add 5 mL of m-cresol to dilute the reaction solution, continue to stir for a few minutes, then pour acetone into it to obtain a flocculent polymer precipitate, filter it, and wash the precipitate repeatedly with acetone several times to remove the residual solvent and unreacted substances, and then dried at 80°C for 25 hours;

[0040] The sulfonated polyimide of the obtained triethyla...

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Abstract

The invention discloses a preparation method of sulfonated polyimide / titanium dioxide composite proton conductive membrane, characterized in that under the protection of nitrogen, 2,2'-disulfonic acid benzidine, meta-cresol and triethylamine are put into a reactor; then 1,4,5,8-naphthalene tetracarboxylic dianhydride, benzoic acid and 4,4' oxydianiline are added, stirred and heated to 70-100 DEG C for reaction for 2-4 hours; then heated to 180-200 DEG C for reaction for 10-20 hours; and then the mixture is cooled and poured into acetone for filtering; the solids are washed by acetone and then dried to obtain sulfonated polyimide of triethylamine salt type. The sulfonated polyimide of triethylamine salt type is dissolved in an organic solvent, and mixed with an organic solvent dispersion liquid of titanium dioxide powder, then casted for filming, and then dried, immersed and washed to obtain sulfonated polyimide proton / titanium dioxide composite proton conductive membrane; the conductive membrane is suitable for an all-vanadium redox flow battery and a fuel cell with good performance.

Description

technical field [0001] The invention belongs to a method for preparing a battery separator, and relates to a method for preparing a sulfonated polyimide / titanium dioxide composite proton conductive membrane. The sulfonated polyimide / titanium dioxide composite proton conductive membrane prepared by the invention can be applied in the fields of all-vanadium redox flow battery, hydrogen-oxygen fuel cell, direct methanol fuel cell and the like. Background technique [0002] Vanadium redox flow battery (Vanadium Redox Flow Battery, referred to as: VRB) is a new type of green secondary battery proposed by Skyllas-Kazacos in 1985. Long, easy to operate and maintain. As a large-scale energy storage system composed of a single metal ion (vanadium ion) for positive and negative redox pairs, it avoids the electrolyte cross-contamination problem of other flow batteries such as Fe / Cr batteries and Na / S batteries. Generally, VRB can be applied to peak-shaving power supply systems, large...

Claims

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Application Information

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IPC IPC(8): C08J7/14C08J5/22C08L79/08C08K3/22C08G73/10
Inventor 张亚萍李劲超王磊张帅
Owner SOUTHWEAT UNIV OF SCI & TECH
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