Sulfonated polyarylether based on triphenylphosphine oxide structure unit and preparation method thereof

A technology of triphenylphosphine oxide and sulfonated polyarylether, which is applied in the field of sulfonated polyarylether based on triphenylphosphine oxide structural unit and its preparation, can solve the problems not involving sulfonated polyarylether, and achieve The synthesis method is simple, the thermal stability is good, and the effect of mild conditions

Inactive Publication Date: 2009-06-03
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this document does not relate to the preparation of the sulf...

Method used

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  • Sulfonated polyarylether based on triphenylphosphine oxide structure unit and preparation method thereof
  • Sulfonated polyarylether based on triphenylphosphine oxide structure unit and preparation method thereof
  • Sulfonated polyarylether based on triphenylphosphine oxide structure unit and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: 3.0mmol bis(4-fluorophenyl)-3'-sulfonate sodium phenylphosphine oxide, 3.0mmol 9,9-bis(4-hydroxyphenyl)fluorene, 3.3mmol cesium carbonate, 8mL1- Methyl-2-pyrrolidone and 9 mL of toluene were added to a three-neck flask equipped with a stirrer, a water separator and a condenser. Under the protection of nitrogen, the temperature was raised to 160°C, and after azeotropic dehydration for 4 hours, the azeotropic dehydrating agent toluene was discharged, the temperature was raised to 175°C, and the reaction was carried out for 60 hours. After natural cooling, precipitate in ethanol and water, desalt after filtration, and vacuum dry at 100°C for 24 hours to obtain sulfonated polyarylether containing triphenylphosphine oxide structural unit.

[0039] The yield of the reaction is 96%, the temperature of 5% thermal weight loss of the product is 385 DEG C, and no glass transition occurs in the range of 100-350 DEG C. The intrinsic viscosity at 30°C was 1.17 dL / g. figu...

Embodiment 2

[0040] Example 2: 1.8mmol bis(4-fluorophenyl)-3'-sulfonate sodium phenylphosphine oxide, 1.2mmol bis(4-fluorophenyl)phenylphosphine oxide, 3.0mmol9,9-bis(4 -Hydroxyphenyl)fluorene, 3.3 mmol of cesium carbonate, 8 mL of 1-methyl-2-pyrrolidone and 9 mL of toluene were added to a three-neck flask equipped with a stirrer, a water separator and a condenser. Under nitrogen protection, the temperature was raised to 150°C, and after azeotropic dehydration for 3 hours, the azeotropic dehydrating agent toluene was discharged, the temperature was raised to 190°C, and the reaction was carried out for 48 hours. After natural cooling, it precipitates in water, desalts after filtration, and vacuum-dries at 100°C for 24 hours to obtain sulfonated polyarylene ether containing triphenylphosphine oxide structural unit.

[0041] The yield of the reaction is 95%, the temperature of 5% thermal weight loss of the product is 411 DEG C, and no glass transition occurs in the range of 100-350 DEG C. Th...

Embodiment 3

[0042]Example 3: 2.7mmol bis(4-fluorophenyl)-3'-sulfonate sodium phenylphosphine oxide, 0.3mmol bis(4-fluorophenyl)phenylphosphine oxide, 3.0mmol 2,2-bis- (4-Hydroxyphenyl)hexafluoropropane, 3.3 mmol of potassium carbonate, 8 mL of 1-methyl-2-pyrrolidone and 8 mL of toluene were added to a three-neck flask equipped with a stirrer, a water separator and a condenser. Under the protection of nitrogen, the temperature was raised to 150°C, and after azeotropic dehydration for 4 hours, the azeotropic dehydrating agent toluene was discharged, the temperature was raised to 185°C, and the reaction was carried out for 80 hours. After natural cooling, it precipitates in water, desalts after filtration, and vacuum-dries at 100°C for 24 hours to obtain sulfonated polyarylene ether containing triphenylphosphine oxide structural unit.

[0043] The yield of the reaction is 96%, the temperature of 5% thermal weight loss of the product is 440°C, and the glass transition temperature is 380°C. T...

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Abstract

The invention discloses sulfonated polyarylether based on a triphenylphosphine oxide structure unit and a preparation method thereof in the technical field of chemical industry. Sulfonated triphenylphosphine monomer, triphenylphosphine monomer and dihydroxyl monomer are used as raw materials to be polycondensed directly in polar solvent by the action of reaction accelerant to obtain a polymer with a structural formula as above, wherein, M is hydrogen ion, lithium ion, sodium ion, kalium ion, cesium ion or ammonium ion; when m is equal to 1, the polymer is a homopolymer containing sulfonated triphenylphosphine oxide; when m is more than 0 and less than 1, the polymer is the multipolymer containing the sulfonated triphenylphosphine oxide. The polymer has good thermal stability, mechanical property and solubility, large molecular weight and good compatibility with inorganic material and can be applied in proton exchange membrane fuel cell field.

Description

technical field [0001] The invention relates to a polymer in the technical field of chemical engineering and a preparation method thereof, in particular to a sulfonated polyarylether based on a triphenylphosphine oxide structural unit and a preparation method thereof. Background technique [0002] Proton exchange membrane is the key material of proton exchange membrane fuel cell. The currently widely used Nafion perfluorinated membrane has some technical defects, such as low electrical conductivity, high methanol permeability, and high price when the temperature is high and the humidity is low. In recent years, the preparation of sulfonated non-fluorinated polyarylethers that can be used in proton exchange membranes has received extensive attention. Sulfonated polyarylether series polymers mainly include polyarylether ketone, polyarylether sulfone, polyphenylene ether, polyphenylene sulfide and their derivatives, which have excellent thermal stability, mechanical strength, ...

Claims

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Application Information

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IPC IPC(8): C08G65/40
Inventor 张春杰桂龙勇马旭辉肖谷雨颜德岳
Owner SHANGHAI JIAO TONG UNIV
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