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Preparation method of polycyclohexene phosphonic acid composite film

A technology of polycyclohexene phosphonic acid and cyclohexene phosphonic acid, which is applied in fuel cell parts, fuel cells, electrical components, etc., and can solve problems such as high price, high methanol penetration rate, and degradation of proton conductivity , achieve the effect of low price and simple preparation process

Inactive Publication Date: 2012-11-07
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The acid-base composite proton exchange membrane prepared by this method has good comprehensive properties, and the preparation method has not been reported in domestic and foreign patents and other documents.

Method used

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  • Preparation method of polycyclohexene phosphonic acid composite film
  • Preparation method of polycyclohexene phosphonic acid composite film
  • Preparation method of polycyclohexene phosphonic acid composite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In this example, polycyclohexene phosphonic acid was synthesized by high-temperature polymerization, and acid-base composite membrane was prepared with polyamide-imide (PAI) as the basic component .

[0024] A. Synthesis of Cyclohexene Phosphonic Acid Monomer

[0025] First, add 0.1 mol (10.4 mL) cyclohexanone and 0.1 mol (8.7 mL) phosphorus trichloride in turn into a dry three-necked flask protected by nitrogen. Next, the reaction was stirred at room temperature for 24 hours under the condition of reflux condensation. Third, slowly add 100 mL of acetic acid with a constant pressure dropping funnel, continue the reaction for 24 hours, and absorb a large amount of hydrogen chloride gas generated during the reaction with sodium hydroxide solution. The 4th, after the reaction finishes, change the condensing reflux device into the circulating water pump decompression distillation device, respectively at 70 o C reduced pressure distillation for 3 hours, 100 o C vacuum d...

Embodiment 2

[0031] In this example, polycyclohexene phosphonic acid was synthesized by high-temperature polymerization, and an acid-base composite film was prepared with polyimide (PI) as the basic component.

[0032] A. Synthesis of Cyclohexene Phosphonic Acid Monomer

[0033]First, add 0.1 mol (10.4 mL) cyclohexanone and 0.1 mol (8.7 mL) phosphorus trichloride in turn into a dry three-necked flask protected by nitrogen. Next, the reaction was stirred at room temperature for 24 hours under the condition of reflux condensation. Third, slowly add 100 mL of acetic acid with a constant pressure dropping funnel, continue the reaction for 24 hours, and absorb a large amount of hydrogen chloride gas generated during the reaction with sodium hydroxide solution. Fourth, after the reaction finishes, change the condensing device into a circulating water pump decompression distillation device, respectively at 70 o C reduced pressure distillation for 3 hours, 100 o C vacuum distillation 0.5 hour...

Embodiment 3

[0039] In this example, ammonium persulfate was used as an initiator to synthesize polycyclohexene phosphonic acid by radical polymerization, and an acid-base composite film was prepared with polyimide (PI) as a basic component.

[0040] A. Synthesis of Cyclohexene Phosphonic Acid Monomer

[0041] First, add 0.05 mol (5.2 mL) cyclohexanone and 0.05 mol (4.4 mL) phosphorus trichloride in turn into a dry three-necked flask protected by nitrogen. Next, the reaction was stirred at room temperature for 24 hours under the condition of reflux condensation. Third, slowly add 50 mL of acetic acid with a constant pressure dropping funnel, continue the reaction for 24 hours, and absorb a large amount of hydrogen chloride gas generated during the reaction with sodium hydroxide solution. Fourth, after the reaction finishes, change the condensing device into a circulating water pump decompression distillation device, respectively at 70 o C reduced pressure distillation for 3 hours, 100 ...

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Abstract

The invention relates to a preparation method of a polycyclohexene phosphonic acid composite film for a fuel cell. The preparation method comprises a method for synthesizing polycyclohexene phosphonic acid monomers by taking cyclohexanone and phosphorus trichloride as raw materials, a method for polymerizing the polycyclohexene phosphonic acid monomers in two manners of high-temperature polymerization and radical polymerization and a method for preparing the polycyclohexene phosphonic acid composite film with a tape casting method. The preparation method provided by the invention is mainly characterized in that prepared polycyclohexene phosphonic acid is an acidic polymer and can be compounded with various alkaline polymers such as polyimide, polyamideimide, polybenzimidazole and the like to prepare an acid-alkali composite proton exchange film with a honeycomb structure. The preparation method is also characterized in that the acid-alkali composite film based on the polycyclohexene phosphonic acid still maintains better proton electroconductivity under a high-temperature anhydrous condition, the acid-alkali composite film which is not subjected to wet processing at 180 DEG C has the electricconductivity of 2.7*10-3-6.4*10-2 mS / cm, and can serve as a high-temperature proton exchange film.

Description

technical field [0001] The invention relates to the technical field of proton exchange membrane fuel cells, in particular to a preparation method of polycyclohexene phosphonic acid, a proton exchange membrane material used in proton exchange membrane fuel cells, and an acid-alkali composite membrane. Background technique [0002] Proton exchange membrane fuel cell (PEMFC) is a type of fuel cell that has been widely studied and has been widely used in aerospace, military, new energy vehicles and other fields. Proton exchange membrane and electrocatalyst are the core materials of proton exchange membrane fuel cell. At present, the most successful proton exchange membrane with the best comprehensive performance is the perfluorosulfonic acid proton exchange membrane represented by DuPont's NAFION membrane. However, the high price of perfluorosulfonic acid proton exchange membranes, high methanol permeability, and severe degradation of proton conductivity at high temperature or ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/22C08L45/00C08L79/08C08L79/04C08F132/04H01M8/02H01M2/16H01M8/1018H01M8/1041
CPCY02E60/12Y02E60/50
Inventor 严六明邸素清张冬芳陈晋冯庆霞
Owner SHANGHAI UNIV
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