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Novel segmented copolymer and preparation method thereof

A technology of block copolymers and oligomers, applied in the direction of final product manufacturing, sustainable manufacturing/processing, electrical components, etc., can solve the problems of reduced production cost, low activity, long reaction time, etc.

Active Publication Date: 2012-07-04
ENN SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the preparation method of the block copolymer of the present invention, the defects of high reaction temperature and long reaction time caused by the low activity of 4,4'-biphenylbisphenol that exist in the above-mentioned prior art that can be solved can be greatly reduced. The small reaction cycle reduces the industrial production cost and is conducive to large-scale promotion

Method used

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  • Novel segmented copolymer and preparation method thereof
  • Novel segmented copolymer and preparation method thereof
  • Novel segmented copolymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0070] 1.1 Synthesis of hydrophobic oligomer 6FBisAF

[0071] In a 100mL three-neck flask equipped with a thermometer, a nitrogen pipe, a condensing water separator, and a stirrer, first add 20mL of N-methylpyrrolidone, then add hexafluorobisphenol A (2.29g, 6.82mmol), and then add potassium carbonate (1.18g, 8.53mmol), then add 10mL toluene, start stirring, raise the temperature to 150°C, the system is azeotropic at this temperature, react at this temperature for 2 hours to remove the water in the system, and then steam the reaction system Toluene in. Then the temperature was lowered to 50°C, and perfluorobiphenyl (2.39g, 7.16mmol) was added, and the reaction was heated up to 100°C, and reacted at this temperature for 3.5 hours. Then the reaction was cooled to room temperature, and the polymer was poured into a mixture of 400mL methanol and water (volume ratio methanol / water=1:1), left to stand for 10 minutes, stirred for another five minutes, filtered, washed twice with wat...

Embodiment 2

[0089] The block copolymer of the present invention is prepared by the same method as in Example 1, except that: in step (1), the hydrophobic oligomer 6FBi sAF is made of perfluorobiphenyl and hexafluorobisphenol A in a ratio of 1.07:1 The mol ratio synthetic; In the step (2), hydrophilic oligomer BPAS100 is by bisphenol A and 3,3 '-sodium disulfonate base-4,4'-dichlorodiphenyl sulfone according to the mol ratio of 1.1:1 Synthesis; In step (3), the hydrophobic oligomer 6FBi sAF and the hydrophilic oligomer BPAS100 were synthesized at a molar ratio of 1.2:1, and the reaction time was changed to 3 days.

[0090] In the obtained block copolymer of the present invention, m and n were 12 and 11, respectively. The viscosity of the synthesized block copolymer was measured: the reduced viscosity was 0.82dL / g.

Embodiment 3

[0092] The block copolymer of the present invention is prepared by the same method as in Example 1, except that: in step (1), the hydrophobic oligomer 6FBisAF is made of perfluorobiphenyl and hexafluorobisphenol A at a ratio of 1.11:1 Molar ratio is synthesized; In step (2), hydrophilic oligomer BPAS100 is synthesized by bisphenol A and 3,3'-sodium disulfonate base-4,4'-dichlorodiphenyl sulfone in a molar ratio of 1.2:1 ; In step (3), the reaction time becomes 4 days.

[0093] In the obtained block copolymer, m and n were 8 and 9, respectively. The viscosity of the synthesized block copolymer was measured: the reduced viscosity was 0.85dL / g.

[0094] According to the novel block copolymer of the present invention, since the reaction can be carried out at a relatively low temperature and the reaction time is shortened, the cost can be significantly reduced, and it can be widely used in industry. Moreover, the novel block copolymer synthesized by the present invention belongs ...

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Abstract

The invention provides a novel segmented copolymer containing a molecular chain structure expressed in a formula (I) and a preparation method of the novel segmented copolymer. In the formula (I) shown in the specification, m is an integer from 5 to 30, and n is an integer from 4 to 32; the preparation method comprises the following three steps of: (1) reacting decafluorobiphenyl with bisphenol hexafluoride A to form a hydrophobic oligomer expressed in a formula (II) shown in the specification; (2) reacting the bisphenol A with 3, 3'-disulfonate base-4, 4'-diphenyl sulfone dihalide to generate a hydrophilic oligomer which is expressed by a formula (III) shown in the specification; and (3) under heating, carrying out polymerization on the hydrophobic oligomer synthesized in the step (1) and the hydrophilic oligomer synthesized in the step (2) to generate the segmented copolymer containing the molecular chain structure expressed in the formula (I).

Description

technical field [0001] The present invention relates to a novel block copolymer and its preparation method. More specifically, the present invention relates to novel block copolymers obtained by copolymerization for use in proton exchange membranes of fuel cells and methods for their preparation. Background technique [0002] Preparation of high-efficiency proton exchange membrane is one of the core technologies of fuel cells. At present, the commonly used proton exchange membranes in the world are perfluorinated proton exchange membranes, the most representative of which is the Nafion series of perfluorinated proton exchange membranes produced by DuPont of the United States. However, the synthesis process of this kind of membrane is complicated, and the preparation cost is high. When methanol is used in methanol fuel cells, severe permeation will occur, and when the temperature is higher than 100 ° C, the proton conductivity will drop sharply due to severe water loss. The...

Claims

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Application Information

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IPC IPC(8): C08G65/00C08G65/40H01M2/16H01M8/02
CPCY02E60/12Y02E60/50Y02P70/50
Inventor 裴增楷李冬杰胡利彦徐世义汪国庆
Owner ENN SCI & TECH DEV
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