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Method for manufacturing a sulfonated poly(1,3,4-oxadiazol) polymer

A technology of polymer and oxadiazole, applied in the field of preparing sulfonated polypolymer, can solve the problems of high cost and reduced proton conductivity, and achieve the effects of good mechanical properties and high proton conductivity

Inactive Publication Date: 2008-12-31
GKSS FORSCHUNGSZENTRUM GEESTHACHT GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disadvantages of this membrane are high cost and reduced proton conductivity at temperatures above 100°C and lower humidity

Method used

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  • Method for manufacturing a sulfonated poly(1,3,4-oxadiazol) polymer
  • Method for manufacturing a sulfonated poly(1,3,4-oxadiazol) polymer
  • Method for manufacturing a sulfonated poly(1,3,4-oxadiazol) polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Synthesis of Sulfonated Poly(1,3,4-oxadiazole)

[0063] direct synthesis

[0064] First, polyphosphoric acid (PPA) was added to the flask and heated to 100°C under a dry nitrogen atmosphere, then hydrazine sulfate salt (HS, >99%, Aldrich) was added to the polyphosphoric acid, homogenized by stirring and heating the reaction medium qualitative.

[0065] After reaching the reaction temperature, Dicarboxyldiazid 4,4'-diphenyl ether, DPE (99%, Aldrich) was added to the flask. The molar dilution ratio (PPA / HS) and molar monomer ratio (HS / DPE) were kept constant at 10 or 1.2. The molar dilution ratio (PPA / HS) and molar monomer ratio (HS / DPE) were chosen based on previous studies to optimize poly(ether-1,3,4-oxadiazole) synthesis with the aid of statistical experimental design (Gomes et al., 2001, supra).

[0066] After 6 hours of reaction of DPE and HS, the reaction medium was added to water containing 5% w / v sodium hydroxide (99%, Vetec) to allow precipitation of the pol...

Embodiment 2

[0084] Water Absorption and Oxidation Stability

[0085] The film was dried at 80° C. in vacuum for 24 hours before measurement. After measuring the weight of the dried film, the samples were immersed in deionized water at 25°C and 60°C for 24 hours.

[0086] Before measuring the weight of the hydrated membrane, wipe off the water from the surface of the membrane with a paper towel. Water absorption is calculated according to the following formula:

[0087] Water absorption (weight%) = (m 湿 -m 干燥 ) / m 干燥 x100,

[0088] where m 湿 and m 干燥 are the dry and hydrated film weights.

[0089] The oxidative stability of the membrane was investigated, wherein the membrane was subjected to Fenton's reagent (containing 2ppm FeSO 4 3% H 2 o 2 ) at 80°C for 1 hour. The results are shown in Table 1.

[0090] Table 1: Water absorption and oxidation stability of sulfonated poly(1,3,4-oxadiazole) membranes

[0091]

[0092] aAccording to elemental analysis

[0093] b Data from ...

Embodiment 3

[0100] Measurement of proton conductivity

[0101] Proton conductivity by frequency between 10 and 10 6 Impedance spectra between Hz are measured with signal amplitudes ≤ 100 mV and determined from the impedance modulus at the high frequency side where the phase shift disappears. The proton conductivity of the samples was measured at 80°C and 15% to 100% relative humidity. Impedance measurements were performed on stacks of up to 5 films, where each stack had a similar overall thickness of about 500 μm. The relative humidity is controlled by blowing nitrogen through the water, heating the water at a suitable temperature between 20°C and 80°C.

[0102] image 3 The proton conductivity of sulfonated poly(1,3,4-oxadiazole) membranes is plotted as a function of temperature. The film has S / C = 0.124, measured at 80°C and 15% to 100% relative humidity.

[0103] image 3 It was shown that a high proton conductivity is achieved, which can be explained inter alia by the structure ...

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Abstract

The invention relates to a method for preparing sulfonic poly(1,3,4-oxadiazole)polymer, also relates to the sulfonic poly(1,3,4-oxadiazole)polymer used for fuel cell membranes, fuel cells and a method for producing the fuel cell. The method includes steps: mixing hydrazine sulfate with one or more dicarboxylic acids or derivatives thereof in polyphosphoric acid to prepare a solution, heating the solution in inert atmosphere, settling the polymer in an alkali solution.

Description

technical field [0001] The present invention relates to a process for preparing sulfonated poly(1,3,4-oxadiazole) polymers. The invention also relates to sulfonated poly(1,3,4-oxadiazole) polymers, membranes for fuel cells, fuel cells and methods for preparing fuel cells. Background technique [0002] Fuel cells require proton-conducting membranes. Such a membrane is, for example, a polymer electrolyte membrane (PEM). A known PEM based on a perfluorocarbon polymer electrolyte membrane is the Nafion membrane developed by DuPont (JP 112 04 119 A). [0003] There are two types of PEM fuel cells under development, low temperature cells, which operate at temperatures up to about 90°C, and high temperature cells, which operate at temperatures up to about 180°C. [0004] Nafion membranes do not have sufficient heat resistance so that the membranes cannot be used at temperatures exceeding 80° C. (see also US 4 330 654). Low temperature fuel cells are sensitive to carbon monoxide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/08H01M8/02H01M2/16
CPCC08G73/08C08J5/2256C08J2379/06H01M8/1004H01M8/1011H01M8/1013H01M8/1027H01M8/103H01M8/1067H01M8/1072H01M2300/0082Y10T29/49108Y02E60/50Y02P70/50C08G61/12C08G73/00C08G75/00
Inventor 多米尼克·德·菲格雷多·戈梅斯耶路撒·罗德·赫苏斯苏珊娜·努内斯
Owner GKSS FORSCHUNGSZENTRUM GEESTHACHT GMBH
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