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Preparation and Application of a Highly Crosslinked and Highly Sulfonated Sulphonated Aromatic Block Polymer Membrane

A block polymer and sulfonated aromatic technology, which is applied in membrane, membrane technology, semi-permeable membrane separation, etc., can solve the problem of consumption of polymer sulfonic acid group content, decrease of proton conductivity, and restriction of sulfonated aromatic block polymerization To improve the mechanical strength and physical and chemical stability, improve the transmission performance, and promote the transmission performance.

Active Publication Date: 2021-04-20
XI AN JIAOTONG UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the performance of sulfonated aromatic block polymers directly depends on the content of its sulfonic acid groups, this crosslinking method consumes the content of polymer sulfonic acid groups, thus affecting its performance
For example, CN200910233400.6 patent improves the anti-swelling performance of the material by thermally crosslinking the linear sulfonated aromatic polymer film. Due to thermal crosslinking, -SO 3 The loss of H reduces the ion exchange capacity of the polymer by about 75%, affecting its application in fuel cells
Literature (M.L.Di Vona,E.Sgreccia,S.Licocccia,etal.Analysis of temperature-promoted and solvent-assisted cross-linking insulfonated poly(ether ether ketone)(S-PEEK)proton-conducting membranes[J].Journal of physical chenmistry B,2009,113:7507–7512) cross-linked sulfonated polyetheretherketone membrane by thermal cross-linking, and found that although the anti-swelling and mechanical properties of the membrane were improved after cross-linking, due to With the consumption of sulfonic acid groups, the proton conductivity drops significantly
At present, the degree of sulfonation of sulfonated aromatic polymer membranes cross-linked by sulfonic acid groups has been greatly reduced, which seriously restricts the application of sulfonated aromatic block polymer membranes in the fields of proton exchange membranes for fuel cells, water treatment, and air dehumidification. Development and Application

Method used

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  • Preparation and Application of a Highly Crosslinked and Highly Sulfonated Sulphonated Aromatic Block Polymer Membrane
  • Preparation and Application of a Highly Crosslinked and Highly Sulfonated Sulphonated Aromatic Block Polymer Membrane
  • Preparation and Application of a Highly Crosslinked and Highly Sulfonated Sulphonated Aromatic Block Polymer Membrane

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[0036] One embodiment of the present invention provides a method for preparing a benzene ring cross-linked sulfonated aromatic block polymer, comprising the following steps:

[0037] a. Dissolve the block polymer in 1,2-dichloroethane solution to prepare a polymer solution with a mass fraction of 0.5 to 10%, and then add a mass fraction of 10 to 30% at 20 to 60°C. Solvent (cyclohexane, cycloheptane or toluene), after adding a co-solvent, then add a sulfonating agent (acetosulfonate, oleum or sulfur trioxide) with a mass fraction of 0.1 to 20%, at 25 to After reacting at 60°C for 1-72 hours, the sulfonated product was precipitated, washed with deionized water until neutral, and finally dried in a vacuum oven at 40-80°C to constant weight to obtain a dried sulfonated aromatic block polymer. Then, the sulfonated aromatic block polymer and the casting solution solvent (one or more of tetrahydrofuran, toluene or hexanol) are formulated into a sulfonated aromatic block polymer solu...

Embodiment 1

[0049] Example 1: The block polymer used is a diblock polymer polystyrene-hydroquinone (SP), wherein x=600, y=300, z=m=0, n=6, M is sub- methyl.

[0050] (1) Sulfonation reaction: Dissolve 1g of block polymer SP in 1,2-dichloroethane solution to prepare a polymer solution with a mass fraction of 5wt%, and then add a mass fraction of 15% at 60°C Cyclohexane, after adding cyclohexane, then add sulfonating agent acetylsulfonate with a mass fraction of 0.1%, react at 60°C for 36 hours, precipitate the sulfonated product, and then wash with deionized water until neutral, Finally, it was dried in a vacuum oven at 80° C. to a constant weight to obtain a dried sulfonated aromatic block polymer. Then the sulfonated aromatic block polymer, toluene and hexanol with a mass ratio of 1:28:4 were formulated into a 3% sulfonated aromatic block polymer solution with a mass fraction, and after complete dissolution, the Perform casting to form a film.

[0051] (2) Cross-linking reaction: add ...

Embodiment 2

[0053] Example 2: The block copolymer used is a tetrablock polymer polystyrene-isobutylene-ethylene-styrene (SBES), wherein x=m=600, y=n=0, z=200, M is methylene base.

[0054] (1) The aromatic block polymer is dissolved in 1,2-dichloroethane to prepare a block polymer solution with a mass fraction of 5%, and after it is completely dissolved, it is poured on a polytetrafluoroethylene plate to form a film. Immerse 2g of block polymer membrane in sulfur trioxide, a sulfonating agent with a mass fraction of 10%, and react at 45°C for 1 hour, then wash the sulfonated membrane with deionized water until neutral to obtain sulfonated aromatic block polymer physical film.

[0055] (2) Cross-linking reaction: add cross-linking agent dimethoxymethane to 60mL 1,2-dichloroethane to prepare a cross-linking agent with a mass fraction of 25%, and then add a catalyst with a mass fraction of 1%. ferric chloride to obtain a mixed solution. The sulfonated aromatic block polymer membrane obtai...

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Abstract

The invention discloses the preparation and application of a sulfonated aromatic block polymer membrane with high crosslinking and high sulfonation degree. In the present invention, the sulfonated aromatic block polymer film is obtained by reacting the styrene block polymer, cosolvent and sulfonating agent; preparing a crosslinking agent and adding a catalyst; immersing the sulfonated aromatic block polymer film in the crosslinking agent , segmented cross-linking; wash off the impurities on the surface of the membrane to obtain a benzene ring cross-linked sulfonated aromatic block polymer membrane. Through the cross-linking modification of the sulfonated aromatic block polymer membrane, the benzene ring is used as the cross-linking site, the reaction is controllable, mild and efficient, and the loss of sulfonate groups will not be caused during the reaction process, which is conducive to maintaining the combination of hydrophilic and hydrophobic The water transport channel formed by block microphase separation can significantly improve the mechanical properties and anti-swelling performance of the polymer film, while avoiding the consumption of polymer functional group content and maintaining high water transport performance.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to the preparation and application of a benzene ring cross-linked sulfonated aromatic block polymer membrane. Background technique [0002] The sulfonic acid group in the sulfonated aromatic block polymer can form a strong ion-dipole interaction with water. Each of them can be aggregated to form a nanoscale microphase separation structure of hydrophilic regions and hydrophobic regions inside the membrane, and the microphase separation forms channels that are conducive to the transmission of protons and water molecules. The microphase separation structure is closely related to the content of sulfonic acid groups. By adjusting the content of sulfonic acid groups, the size of water molecule transport channels can be adjusted. Higher content of sulfonic acid groups has higher water transport capacity. At a high degree of sulfonation, the sulfonic acid groups can be connecte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/22C08J3/24C08L53/00C08L53/02C08L87/00C08K5/06C08K5/053B01D71/76B01D69/02B01D67/00C02F1/44B01D53/26H01M8/1088H01M8/1023H01M8/1025
CPCB01D53/268B01D67/0006B01D69/02B01D71/76B01D2325/42C02F1/44C08J3/24C08J5/2243C08J5/225C08J5/2268C08J5/2287C08J5/2293C08J2353/00C08J2353/02C08J2387/00C08K5/053C08K5/06H01M8/1023H01M8/1025H01M8/1088Y02E60/50Y02P70/50
Inventor 李娜延檬羽边文海曾飞祥
Owner XI AN JIAOTONG UNIV