Microporous carbon fiber material prepared from polyacrylonitrile and used for high-selectivity separation of various micromolecular gases, and preparation method and application of microporous carbon fiber material

A technology of polyacrylonitrile and fiber materials, applied in the field of microporous carbon fiber materials and its preparation, to achieve excellent industrial application prospects, good chemical stability and hydrothermal stability, and narrow pore size distribution

Active Publication Date: 2022-04-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, there are few reports on the separation of the above multiple gas systems by adjusting the synthesis parameters of the same series of materials.

Method used

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  • Microporous carbon fiber material prepared from polyacrylonitrile and used for high-selectivity separation of various micromolecular gases, and preparation method and application of microporous carbon fiber material
  • Microporous carbon fiber material prepared from polyacrylonitrile and used for high-selectivity separation of various micromolecular gases, and preparation method and application of microporous carbon fiber material
  • Microporous carbon fiber material prepared from polyacrylonitrile and used for high-selectivity separation of various micromolecular gases, and preparation method and application of microporous carbon fiber material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] 1 g of polyacrylonitrile and 9 g of N,N-dimethylformamide were stirred and mixed at 40° C. for 24 h, and then 0.5 g of anhydrous zinc chloride was added. The mixed solution was stirred at 30°C under airtight conditions for 8 hours to make it uniformly dispersed. Then the mixed solution was subjected to electrospinning, the spinning voltage was 18KV, the injection rate was 1.0ml / h, the distance between the needle and the collector was 12cm, and the spinning time was 20h. After the polymer fibers obtained by spinning were dried at 150°C for 8 hours, 0.3 g was added to 25 ml of ethylene glycol, and while stirring at 130°C, 0.12 ml of ethylenediamine was added dropwise, reacted for 3 hours, and then suction-filtered to obtain crosslinked fibers. After the product is dried, put it in a porcelain boat, put it into a high-temperature tube furnace, and control the heating rate at 5°C / min under a nitrogen atmosphere. After rising to 800°C, perform an activation reaction for 1 ho...

Embodiment 2

[0067] 1 g of polyacrylonitrile and 9 g of N,N-dimethylformamide were stirred and mixed at 30° C. for 24 h, and then 0.5 g of anhydrous zinc chloride was added. The mixed solution was stirred at 30°C under airtight conditions for 8 hours to make it uniformly dispersed. Then the mixed solution was subjected to electrospinning, the spinning voltage was 20KV, the injection rate was 0.8ml / h, the distance between the needle and the collector was 10cm, and the spinning time was 20h. After drying the polymer fiber obtained by spinning at 130°C for 10 hours, take 0.5g and add it to 25ml of glycerol, while stirring at 135°C, add 0.25ml of 1,2-propylenediamine dropwise, react for 3 hours, and then filter with suction to obtain Cross-linked fibers. After the product is dried, put it in a porcelain boat, put it into a high-temperature tube furnace, and control the heating rate at 5°C / min under a nitrogen atmosphere. After rising to 800°C, perform an activation reaction for 1 hour to obta...

Embodiment 3

[0069] 1 g of polyacrylonitrile and 9 g of N,N-dimethylformamide were stirred and mixed at 30° C. for 24 h, and then 1.0 g of anhydrous zinc acetate was added. The mixed solution was stirred at 30°C under airtight conditions for 8 hours to make it uniformly dispersed. Then the mixed solution was subjected to electrospinning, the spinning voltage was 20KV, the injection rate was 0.8ml / h, the distance between the needle and the collector was 10cm, and the spinning time was 20h. After the polymer fibers obtained by spinning were dried at 120°C for 12 hours, 0.5 g was added to 25 ml of propylene glycol, and while stirring at 135°C, 0.4 ml of ethylenediamine was added dropwise, reacted for 3 hours, and suction filtered to obtain crosslinked fibers. After the product is dried, put it in a porcelain boat, put it into a high-temperature tube furnace, and control the heating rate at 5°C / min under a nitrogen atmosphere. After rising to 900°C, perform an activation reaction for 1 hour to...

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Abstract

The invention provides a microporous carbon fiber material prepared from polyacrylonitrile and used for high-selectivity separation of various micromolecular gases, and a preparation method and application thereof. The preparation method comprises the following steps: (1) preparation of polyacrylonitrile fibers: uniformly stirring polyacrylonitrile and N, N-dimethylformamide at 30-60 DEG C, adding a metal salt activator, uniformly stirring, then carrying out electrostatic spinning, and drying to obtain polymer fibers; (2) cross-linking the fibers: dropwise adding a cross-linking agent into the polymer fibers obtained in the step (1) while stirring at 80-140 DEG C to obtain cross-linked fibers; and (3) carbonization and activation: placing the cross-linked fiber obtained in the step (2) in an inert atmosphere, and carrying out a high-temperature activation reaction at 600-900 DEG C to obtain the microporous carbon fiber material. The microporous carbon fiber material prepared by the preparation method disclosed by the invention has excellent performance in a system for separating multiple small molecule gases, and has a good industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of small molecule gas separation, in particular to a microporous carbon fiber material prepared by polyacrylonitrile for highly selective separation of various small molecule gases, a preparation method and an application thereof. Background technique [0002] High-purity small molecule gases, including methane (CH 4 ), carbon dioxide (CO 2 ), nitrogen (N 2 ), oxygen (O 2 ), xenon (Xe), krypton (Kr), fluoromethane (CH 3 F), etc., are important industrial gases in the national economic system. As the clean fuel with the highest H / C ratio and high calorific value, methane has proven reserves of more than 250 trillion cubic meters in the world, and is widely found in conventional gas sources such as coalbed methane and shale gas and unconventional gas sources such as biogas and landfill gas . The main components of conventional gas sources are methane and nitrogen. The presence of nitrogen greatly affects...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01F1/10B01D53/02C10L3/10
CPCD01F9/22D01F1/10B01D53/02C10L3/104C10L3/105B01D2257/504B01D2257/102
Inventor 肖静黄佳武杜胜君廖能
Owner SOUTH CHINA UNIV OF TECH
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