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A kind of hypercrosslinked porous polymer fiber and preparation method

A porous polymer and hypercrosslinking technology, applied in the direction of single-component synthetic polymer rayon, chemical post-processing of synthetic polymer rayon, chemical characteristics of fibers, etc. It is suitable for large-scale preparation and other problems, and achieves the effect of large aspect ratio and high specific surface area

Active Publication Date: 2022-07-26
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Or prepare a bottle brush copolymer precursor by organic synthesis, use its main chain as a template, and a large number of aromatic rings in its side chains are woven under the action of an external linking agent to form a hypercrosslinked structure to obtain hypercrosslinked polymer fibers , but this method requires the use of RAFT to control polymerization during the preparation process, which is technically difficult and has low preparation efficiency, and is not suitable for large-scale preparation (Polym.Chem., 2016, 7, 4975)
At present, there is no report on the synthesis of hypercrosslinked polymer fibers by a simple one-step method using aromatic macromolecules as monomers. This invention is expected to further enrich the synthesis methods of hypercrosslinked polymer fibers

Method used

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  • A kind of hypercrosslinked porous polymer fiber and preparation method
  • A kind of hypercrosslinked porous polymer fiber and preparation method
  • A kind of hypercrosslinked porous polymer fiber and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1: Preparation of Hypercrosslinked Porous Polymer Fibers

[0028] Under ultrasonic assistance, 0.8 g of monomer 1 was dissolved in 18 mL of 1,2-dichloroethane to obtain solution I, and 0.4 g of anhydrous ferric chloride was dissolved in 8 mL of 1,2-dichloroethane to obtain a solution II; add 150mL of dimethyl silicone oil with a viscosity of 100cs to a 250mL three-necked flask and place it in an oil bath, heat up to 42°C, under 350r / min mechanical stirring, add solution I and solution II to the three-necked flask in turn, and Stir for 5h; raise the temperature of the system to 82°C, continue the reaction for 8h, cool down to room temperature after the reaction, separate the product by suction filtration, wash twice with 1,2-dichloroethane and extract with ethanol for 24h, dry Then, hypercrosslinked porous polymer fibers are obtained.

Embodiment 2

[0029] Example 2: Preparation of Hypercrosslinked Porous Polymer Fibers

[0030] Under ultrasonic assistance, 1.5 g of monomer 2 was dissolved in 30 mL of 1,2-dichloroethane to obtain solution I, and 0.5 g of anhydrous aluminum trichloride was dissolved in 20 mL of 1,2-dichloroethane to obtain a solution II; add 300mL of dimethyl silicone oil with a viscosity of 50cs to a 500mL three-necked flask and place it in an oil bath, heat up to 42°C, under 300r / min mechanical stirring, add solution I and solution II to the three-necked flask in turn, and Stir for 4h; raise the temperature of the system to 82°C, continue the reaction for 10h, cool down to room temperature after the reaction, separate the product by suction filtration, wash twice with 1,2-dichloroethane and extract with ethanol for 24h, dry Then, hypercrosslinked porous polymer fibers are obtained.

Embodiment 3

[0031] Example 3: Preparation of Hypercrosslinked Porous Polymer Fibers

[0032] Under ultrasonic assistance, 0.25g of monomer 5 was dissolved in 6mL of 1,2-dichloroethane to obtain solution I, and 0.2g of anhydrous ferric chloride was dissolved in 4mL of 1,2-dichloroethane to obtain a solution II; add 60mL of dimethyl silicone oil with a viscosity of 150cs to the 100mL three-necked flask and place it in an oil bath, heat up to 42°C, and under mechanical stirring at 350r / min, add solution I and solution II to the three-necked flask in turn, and Stir for 5h; raise the temperature of the system to 82°C, continue the reaction for 6h, cool down to room temperature after the reaction, separate the product by suction filtration, wash twice with 1,2-dichloroethane and extract with ethanol for 24h, dry Then, hypercrosslinked porous polymer fibers are obtained.

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Abstract

The invention relates to a hypercross-linked porous polymer fiber and a preparation method. The macromonomer and catalyst are dissolved in a good solvent 1,2-dichloroethane, then added to a non-good solvent dimethyl silicone oil, and subjected to Affected by the difference in solubility, macromonomers are precipitated, and filaments are formed under the action of directional stretching by mechanical stirring. Dimethicone oil can separate the stretched filaments, and the liquid filaments can exist stably in the reaction system. , and finally a hypercrosslinking reaction occurs under the action of the catalyst, and the hypercrosslinked porous polymer fibers are formed by curing. This method can realize the rapid synthesis of hypercrosslinked polymer fibers with large size (millimeter-scale length, micron-scale diameter), large aspect ratio, and high specific surface area. Support and other fields can be widely used, and can be converted into porous carbon fibers after carbonization.

Description

technical field [0001] The invention belongs to the field of porous polymer materials, and relates to a hypercrosslinked porous polymer fiber and a preparation method. Background technique [0002] Hypercross-linked polymer is a kind of porous polymer material with bridged network structure formed by rigid aromatic monomer through Fus-gram alkylation reaction. It has light weight, controllable pore structure, large specific surface area, good Therefore, it is widely used in water treatment, heterogeneous catalysis, gas adsorption and separation and other fields. Among them, hypercrosslinked polymer fibers have a one-dimensional structure that is different from granular materials, and are easy to be further assembled into a three-dimensional network by lap entanglement, and their mechanical properties are significantly enhanced, showing more obvious advantages in the application process. Therefore, the development of synthetic methods for hypercrosslinked polymer fibers is o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/94D01F1/10D01F11/08D01F9/24
CPCD01F6/94D01F1/10D01F11/08D01F9/24
Inventor 张宝亮王继启张云飞刘逸凡温煦刘苏瑶
Owner NORTHWESTERN POLYTECHNICAL UNIV